research article simple atomic absorption spectroscopic...

Research ArticleSimple Atomic Absorption Spectroscopic andSpectrophotometric Methods for Determination of PioglitazoneHydrochloride and Carvedilol in Pharmaceutical Dosage Forms

Afaf A Abdelmonem1 Gamal H Ragab1 Hisham Hashem12 and Eman A Bahgat1

1 Faculty of Pharmacy Pharmaceutical Analytical Chemistry Department Zagazig University Zagazig 44519 Egypt2 Faculty of Pharmacy Pharmaceutical Chemistry Department Jazan University Jazan 45142 Saudi Arabia

Correspondence should be addressed to Hisham Hashem hisham413yahoocom

Received 31 January 2014 Revised 6 April 2014 Accepted 14 April 2014 Published 18 May 2014

Academic Editor Shigehiko Takegami

Copyright copy 2014 Afaf A Abdelmonem et al This is an open access article distributed under the Creative Commons AttributionLicense which permits unrestricted use distribution and reproduction in any medium provided the original work is properlycited

This study represents simple atomic absorption spectroscopic and spectrophotometric methods for determination of pioglitazonehydrochloride (PGZ-HCl) and carvedilol (CRV) based on formation of ion-pair associates between drugs and inorganic complexbismuth(III) tetraiodide (Method A) and between drugs and organic acidic dyes fast green and orange G (Method B) MethodA is based on formation of ion-pair associate between drugs and bismuth(III) tetraiodide in acidic medium to form orange-redion-pair associates which can be quantitatively determined by two different proceduresThe formed ion-pair associate is extractedby methylene chloride dissolved in acetone dried and then decomposed by hydrochloric acid and bismuth content is determinedby direct atomic absorption spectrometric technique (Procedure 1) or extracted by methylene chloride dissolved in acetone andquantified spectrophotometrically at 490 nm (Procedure 2) Method B is based on formation of ion-pair associate between drugsand either fast green dye or orange G dye in acidic medium to form ion-pair associates The formed ion-pair associate is extractedby methylene chloride and quantified spectrophotometrically at 630 nm (for fast green dye method) or 498 nm (for orange G dyemethod) Optimal experimental conditions have been studied Both methods are applied for determination of the drugs in tabletswithout interference

1 Introduction

PGZ-HCl (plusmn)-5-p-[2-(5-ethyl-2-pyridyl) ethoxy] benzyl-24-thiazolidine dione hydrochloride (Figure 1(a)) is athiazolidine-dione oral antidiabetic similar to rosiglitazoneIt is used in the management of type 2 diabetes mellitus Itis given orally as a monotherapy particularly in patients whoare overweight and for whom metformin is contraindicatedor not tolerated [1]

Several spectrophotometric methods have been reportedfor estimation of PGZ-HCl including ion-pair complexformation with bromothymol blue bromophenol blue andbromocresol purple [2] and chlorophenol red [3] as wellas interaction with diazotized sulfanilic acid [4] Derivativespectrophotometry [5] has been also applied An atomic

absorption spectrometric method for determination of PGZ-HCl has been reported which is based on reaction of thedrug with calcium disodium edentate and sodium chlorideto give pink and violet colored metal complexes respectively[6] These complexes are readily extracted with chloroformand determined by atomic absorption spectrometer at 2882and 2277 nm respectively [6] Other methods include flowinjection analysis [7] and voltametry [8] Chromatographicmethods [9ndash11] have been reported such as very rapid separa-tion and quantitation of PGZ-HCl in presence of metformin-HCl onmonolithic column [9] as well as a stability indicatingdensitometric RP-TLC method [10]

CRV (2RS)-1-(9H-carbazol-4-yloxy)-3-[2-(2-methoxy-phenoxy) ethyl]amino-propan-2-ol (Figure 1(b)) is a beta-adrenoceptor antagonist an arteriolar vasodilator that is

Hindawi Publishing CorporationInternational Journal of SpectroscopyVolume 2014 Article ID 768917 17 pageshttpdxdoiorg1011552014768917

2 International Journal of Spectroscopy

O

N

NH

S

O

O

middotHCl

H3C

(a)

OO

NH

HN

H OH

OCH3

And enantiomer

(b)

Figure 1 Chemical structures of (a) PGZ-HCl and (b) CRV

indicated for the treatment of hypertension angina pectorisand heart failure [1]

CRV and its pharmaceutical formulations have beenassayed in BP [14] which describes nonaqueous titrationby dissolving the drug in anhydrous acetic acid and thentitration with 01M perchloric acid determining the end-point potentiometrically Several spectrophotometric meth-ods have been reported for estimation of CRV includingion-pair complex formation with bromocresol green andbromothymol blue as well as charge-transfer reaction ofthe drug with the sigma-acceptor iodine [15] Also UVspectrophotometric determination ofCRV inpharmaceuticalformulations was applied [16ndash18] Other methods includingdetermination of CRV by its quenching effect on the lumi-nescence of terbium complex in dosage form [19] spectroflu-orimetric determination via derivatization with 7-Chloro-4-niritrobenzofurazon [20] and nonaqueous titration [21]have been described Chromatographic methods have beenreported such as validated HPLC determination of the fixeddose combination (CRV and hydrochlorothiazide) in theirtablets [22] HPLC with fluorescence detection [23] and RP-HPLC method for monitoring of the photochemical stabilityof CRV and its degradation products [24] A Chiral HPLC-separation and determination of CRV from human urine wasalso noticed [25] A stability-indicating HPLC-DAD deter-mination of a mixture of carvedilol and hydrochlorothiazide[26] and also UPLC-MSMS method for assay of carvediloland its active metabolite in human plasma were introduced[27] No atomic absorption spectrometricmethods have beenpreviously reported for CRV determination

Bismuth(III)-iodide compounds have been used asreagents for determination of some nitrogenous drugs suchas amineptine hydrochloride piribedil and trimebutinemaleate [28] It has been also used for spectrophotomet-ric and atomic absorption spectroscopic determination ofmoxifloxacin hydrochloride [29] as well as levofloxacinnorfloxacin and ciprofloxacin [30] It has been also usedfor conductometric determination of lomefloxacine HClpantoprazole sodium and sumatriptan succinate [31] Onmixing aqueous solutions of bismuth(III) tetraiodide com-plex and the cited drugs in an acidic medium a reddishorange precipitate instantaneously appeared that is attributedto the ion pair formed in the reaction (Scheme 1)The formedprecipitates are then extracted and quantified spectrophoto-metrically at 490 nm or filtered dried and then decomposed

by hydrochloric acid and the bismuth content is determinedby AAS at 2231 nm [31]

Fast green FCF (Figure 2(a)) is an acidic dye used forspectrophotometric determination of some anthelmintics[32] mebeverine [33] and ceftiofur [34] It has been also usedfor kinetic spectrophotometric determination of trace ruthe-nium [35] and in catalytic analysis of ultratrace rutheniumwith oscillopolarographic detection [36]

OrangeG (Figure 2(b)) is also an acidic dye used for spec-trophotometric determination of citalopram hydrobromidedonepezil hydrochloride rabeprazole sodium [37] fromtablet formulation omeprazole [38] tramadol hydrochloride[39] drotaverine hydrochloride [40] and some antihis-taminic and skeletal muscle relaxant drugs [41] It has beenalso used for spectrophotometric determination of traceruthenium [42] and cationic and anionic surfactants in thepresence of nonionic surfactants [43]

In this paper new and simple atomic absorption spec-troscopic and spectrophotometric methods are proposed fordetermination of some nitrogenous drugs based on theformation of ion pair associated with Bi(III)-iodide complexfast green or orangeG dyesThe proposedmethods have beenapplied to the assay of these drugs in tablets

2 Experiment

21 Apparatus All of the spectrophotometric measurementswere carried out using a Shimadzu UV-1800 with matched1 cm quartz cells (Japan) A Lutron digital pH-meter was usedfor pH adjustment (103 Taipei Taiwan) Shimadzu atomicabsorption spectrophotometric model AA-640-13 was used

22 Materials All solutions were prepared with analytical-grade chemicals and water was always doubly distilled Thestudied drugs were of pharmaceutical grade Standard bis-muth(III) solution 33 times 10minus3M was prepared by dissolving04824 g of bismuth subnitrate (Evans united kingdom) in5mL of conc HNO

3

and adding distilled water and stan-dardized complexometrically [43] 05M potassium iodidewas prepared by dissolving 833 g of KI (Universal finechemicals PVT-LTD India) in 100mL of water Solutions oflower concentration were obtained by accurate dilution ofthese solutions with water Acetic acid hydrochloric acidand sulphuric acid solutions of different molarities wereprepared as in recommended methods [44] Fast green FCF

International Journal of Spectroscopy 3

ONH

S

O

ON

ONH

S

O

ONH

NH

O NH

O

OH

OMe

NH

O

OH

NO

OMe

HH

minus

+

Pioglitazone

Pioglitazone-bismuth tetraiodide ion-pair associate

Carvedilol

Carvedilol-bismuth tetraiodide ion-pair associate

H+

H+

H3C

H3C

+

+

+

Bi(I)4

minus

Bi(I)4

minus

Bi(I)4

minus

Bi(I)4

Scheme 1 Proposed pathway for the reaction between the studied drugs and bismuth tetraiodate

OH

SO3minus

SO3minus

minusO3S

N

N+

(a)

OH

NN

SO3Na

SO3Na

(b)

Figure 2 Chemical structures of (a) fast green FCF and (b) orange-G


(Sigma Chem Company Milwaukee WI USA) was used as001 wv in double distilled water Orange G (Sigma ChemCompany Milwaukee WI USA) was used as 02 wv and04 wv in double distilled water

23 Pharmaceutical Preparations The following availablepharmaceutical preparations were obtained from the Egyp-tian market and analyzed

(i) Diabetin tablets containing 30mg PGZ-HCl pertablet (product of Unipharma El-Obour city Egypt)

(ii) Carvid tablets labeled to contain 25mgCRVper tablet(product of Multi-Apex Pharma Badr city Egypt)

24 Preparation of Standard Drug Solutions

For Method A PGZ-HCl (Unipharma El-Obour city Egypt)stock solution 025mgmLminus1 was prepared by dissolving125mg of PGZ in 5mL of 01M HCI and diluting to 50mLwith water (for both Procedure 1 and Procedure 2)

CRV (Amoun Pharmaceutical Co El-Obour city Egypt)stock solution was prepared by dissolving 50mg of thedrug in methanol and diluting to 100mL with methanol A125mL aliquot of this solution was diluted to 25mL withwater to obtain drug with 025mgmLminus1 concentration (forProcedure 1) Another CRV stock solution was prepared bydissolving 50mg of the drug in methanol and diluting to50mL with methanol A 10mL aliquot of this solution wasdiluted to 25mL with water to obtain drug with 04mgmLminus1concentration (for Procedure 2)

For Method B PGZ-HCl (Unipharma El-Obour city Egypt)working solution 50120583gmLminus1 and for molar ratio 1 times 10minus4Msolution were prepared by dissolving in the least amountof 01M HCl and then completing to volume with distilledwater for fast green FCFmethod while for orange Gmethodworking solution 1000 120583gmLminus1 and for molar ratio 2 times10minus3M solution were prepared by dissolving in the least

amount of 05MH2

SO4

and then completing to volume withdistilled water

CRV (Amoun Pharmaceutical Co El-Obour city Egypt)working solution 50120583gmLminus1 and for molar ratio 1 times 10minus4Msolution were prepared by dissolving in the least amountof methanol and then completing to volume with distilledwater for fast green FCFmethod while for orange Gmethodworking solution 500120583gmLminus1 and for molar ratio 7times10minus4Msolution were prepared by dissolving in the least amount ofmethanol and then completing to volumewith distilledwater

25 General Procedures

251 Construction of Calibration Curves

For Method A

Procedure 1 Specified amounts of 33 times 10minus3M bismuthsubnitrate and 05M KI solutions were placed in a 60mLseparating funnel Different aliquots of PGZ-HCl ranging

from 01 to 1mL of standard working solution and differentaliquots of CRV ranging from 02 to 16mL of standardworking solution were added and pH is adjusted to 24by adding an appropriate amount of HNO

3

(2 vv) Thesolution was completed to 10mL with water in case of PGZ-HCl but no water was added in case of CRV and then 5mLof methylene chloride and 05mL of acetone were added andshaken for 2minutesThe organic layer was filtered through aWhatman no 41 filter paper and dried in boiling water bathThe dried organic phase was dissolved in 05mL Conc HCland the volume was completed to 5mL with double distilledwater A blank omitting the drug was prepared under thesame conditions The bismuth absorbance was measured atthe following conditions

(i) analysis wavelength 223 nm(ii) lamp current 5mA(iii) slit width 38 A(iv) burner height 5mm(v) burner slot flame 10 cm air-C

2

H2

(vi) support gas flow 10 Lminminus1

(vii) fuel gas flow 26 Lminminus1(viii) absorption sensitivity 06 ppm

The concentration of the consumed bismuth was calcu-lated from calibration graph of standard bismuth subnitratesolution

Procedure 2 Specified amounts of 33 times 10minus3M bismuthsubnitrate and 05M KI solutions were placed in a 60mLseparating funnel Different aliquots of PGZ-HCl rangingfrom 03 to 13mL of standard working solution and differentaliquots of CRV ranging from 02 to 09mL of standardworking solution were added and pH is adjusted to 24by adding an appropriate amount of HNO

3

(2 vv) Thesolution was completed to 10mL with water in case of PGZ-HCl but no water was added in case of CRV then 5mLof methylene chloride and 05mL of acetone were addedfor both drugs and shaken for 2 minutes The organic layerwas filtered through a Whatman no 41 filter paper andmeasured at 490 nm against a reagent blank prepared andtreated similarly

For Method B

Fast Green FCF Method Aliquots of standard solutionsranging from 01 to 07 and 01 to 06mL of PGZ-HCl andCRV respectively were transferred into a series of 60mLseparating funnels To each separating funnel 1mL of fastgreen FCF dye (001 wv) was added followed by specificvolumes of acetic acid PGZ-HCl produced intense colorwithout using acetic acidThe formed ionpairswere extractedwith 2 times 5mL of methylene chloride The solutions werevigorously shaken for one minute and the separated organiclayer dried over anhydrous sodium sulphate and transferredinto 10mL volumetric flasks The volumes were completedto 10mL with methylene chloride The absorbance of the


colored solutions was measured at 631 nm against reagentblank treated similarly

Orange GMethod Aliquots of standard solutions rangingfrom 01 to 07 and 02 to 09mL of PGZ-HCl and CRVrespectively were transferred into a series of 60mL separatingfunnels To PGZ-HCl and CRV 05mL of 04 wv and02 wv orange G dye were added respectively followed byspecific volumes of acetic acid PGZ-HCl produced intensecolor without using acetic acid (Table 2) The formed ionpairs were extracted with 2 times 5mL of methylene chlorideThe solutions were vigorously shaken for one minute and theseparated organic layer was dried over anhydrous sodiumsulphate and transferred into 10mL volumetric flasks Thevolumes were completed to 10mL with methylene chlorideThe absorbance of the colored solutions was measured at498 nm against reagent blank treated similarly

252 Procedure for Dosage Forms

(1) Analysis of Diabetin Tablets (PGZ-HCl)

For Method A An accurately weighed amount of the pow-dered tablets equivalent to 25mg of the drug was transferredto a beaker and extracted with 5mL of 01M HCl for 10minand diluted with water The mixture was filtered through afilter paper and washed with water The filtrate and washingwere collected in a 50mL volumetric flask and diluted tovolume with water and then subjected to analysis by therecommended procedure

For Method B

Fast Green FCF Method Weigh and finely powder 10 tabletsExtract an accurately weighed portion of the powder equiv-alent to about 10mg of the drug with 10mL of 01M HClby occasional shaking for 15 minutes Filter the mixture into100mL calibrated flask then wash the residue several timeswith the same solvent and dilute to 100mL with the samesolvent Take 5mL of this stock and dilute to 10mL withdistilled water

OrangeGMethodWeigh and finely powder 10 tablets Extractan accurately weighed portion of the powder equivalent toabout 25mg of the drug with 10mL of 05M H

2

SO4

byoccasional shaking for 15 minutes Filter the mixture into25mL calibrated flask wash the residue several timeswith thesame solvent and dilute to 25mL with the same solvent

(2) Analysis of Carvid Tablets (CRV)

For Method A An accurately weighed amount of the pow-dered tablets equivalent to 50mg of the drug was transferredto a beaker extracted with methanol filtered through a filterpaper and washed with methanol The filtrate and washingwere collected in a 50mL volumetric flask and diluting tovolume with methanol A 10mL aliquot of this solution wasdiluted to 25mLwithwater to obtain 04mgmLminus1 ofCRVandthen subjected to analysis by the recommended procedure

For Method B

Fast Green FCF Method Weigh and finely powder 10 tabletsExtract an accurately weighed portion of the powder equiv-alent to about 25mg of the drug with 10mL of methanolby occasional shaking for 15 minutes Filter the mixture into100mL calibrated flask wash the residue several times withthe same solvent and dilute to 100mL with the same solventTake 10mL of this stock and dilute to 50mL with distilledwater

OrangeGMethodWeigh and finely powder 10 tablets Extractan accurately weighed portion of the powder equivalentto about 50mg of the drug with 10mL of methanol byoccasional shaking for 15 minutes Filter the mixture into50mL calibrated flask wash the residue several timeswith thesame solvent and dilute to 50mLwith the same solvent Take5mL of this stock and dilute to 10mL with distilled water

3 Results and Discussion

31 For Method A Bismuth(III)-iodide compounds havebeen used as reagents for the determination of some nitroge-nous drugs The formation of the ion pair between thesecondary or tertiary amine group of the drug and Bi(III)-iodide binary complex occurs via the protonated nitrogenatom of the drug On mixing aqueous solutions of Bi(III)-iodide complex and the cited drugs in an acidic medium areddish orange precipitate appears that is attributed to the ionpairs formed in the reactionThe extraction of these ion pairswith different solvents was studied Only low-polarity sol-vents such as chloroform methylene chloride and ethylenechloride selectively extract the ion pairs Methylene chloridewas chosen as the extraction solvent because of its higherefficiency and considerable lower extraction ability for thereagent blank Addition of a small amount of acetone provedto be useful Ion pair in methylene chloride was measuredover the wavelength range 400ndash560 nm The ion pair showsmaximum absorbance at 490 nm (Figures 3 and 4) whichcan therefore be used as the wavelength for the analyticaldeterminationThe reagent blank at this wavelength has a lowabsorbance

All measurements were performed against a reagentblank Results are shown in Table 1 Different variables affect-ing the reaction were studied It was not practical to aspiratethe organic solvent of ion pair in the atomic absorptionspectrometer because the high chlorine-carbon ratio wouldlead to the formation of a large quantity of HCl in theframe which would damage the instrument [41] To avoidthis damage ion pair was extracted with organic solventand dried and then the residue was dissolved in conc HClDifferent solvents were tried to dissolve the residue such asconc ammonium hydroxide and conc HCl and it was foundthat conc HCl is the suitable solvent for dissolving the ionpair as it gives maximum solubility and best sensitivity

311 Effect of pH With increasing pH greater than 3 thereis a decrease in extraction yield probably because of pre-cipitation of bismuth as hydroxo-species The absorbance at


Table 1 Characteristic parameters for the reaction of PGZ-HCl and CRV with bismuth tetraiodide via Method Alowast

Parameters PGZ-HCl CRVProcedure 1 Procedure 2 Procedure 1 Procedure 2

120582max (nm) 223 490 223 490Beerrsquos law limits (120583gmLminus1) 5ndash50 15ndash65 10ndash80 16ndash72Vol and conc of bismuth subnitrate of 33 times 10minus3M 03mL 03mL 04mL 04mLVol and conc of potassium iodide of 05M 05mL 05mL 07mL 07mLExtracting solvent Methylene chloride Methylene chloride Methylene chloride Methylene chlorideRegression equationlowastlowast

Slope (119887) 27642 00143 37383 00136Intercept (119886) 10252 00177 55097 minus00932Correlation coefficient (1199032) 09999 09999 09999 09999Molar ratio 1 1 1 1 1 1 1 1

lowastlowast

119860 = 119886 + 119887119862 where 119862 is the concentration of drug in 120583gmLminus1 119860 is the absorbance 119886 is the intercept and 119887 is the slopelowastAverage of three experiments

(a)

(b)

(c)

1000

0500

0000

minus0100

Abso

rban

ce (m

AU)

39999 45000 50000 55000

(nm)

Figure 3 Absorption spectra of (a) the reaction of 50 120583gmLminus1 PGZ-HCl with 03mL of 33 times 10minus3M bismuth subnitrate and 05mLof 05M potassium iodide (b) 03mL of 33 times 10minus3M bismuthsubnitrate and 05mL of 05M potassium iodide and (c) 50120583gmLminus1PGZ-HCl against methylene chloride

120582max remains constant in the pH range of 20ndash28 As theshape of the absorption maximum does not vary with pHit is assumed that in this pH range only one type of ion pairis formed The use of a suitable buffer solution was avoidedbecause the presence of any foreign ion could interfere withthe ion-pair formation hence 2 (vv) of HNO

3

was used toadjust the pH of the solution

312 Effect of Bismuth Subnitrate Volume Different volumesof bismuth subnitrate were added to a fixed concentrationof each drug in the presence of other constituents of theprocedure It was found that 04mL of 33 times 10minus3M bismuthsubnitrate solution for CRV and 03mL for PGZ-HCl weresufficient for the production of maximum and reproduciblecolour intensity (Figure 5)

313 Effect of Potassium Iodide Volume Different volumes ofpotassium iodide were added to a fixed concentration of each

(a)

(b)

(c)

1000

0800

0600

0400

0200

000040000 45000 50000 55000

(nm)

Abso

rban

ce (m

AU)

Figure 4 Absorption spectra of (a) the reaction of 56 120583gmLminus1 CRVwith 04mL of 33 times 10minus3M bismuth subnitrate and 07mL of 05Mpotassium iodide (b) 04mL of 33times10minus3Mbismuth subnitrate and07mL of 05M potassium iodide against methylene chloride and(c) 56 120583gmLminus1 CRV against methylene chloride

drug in the presence of other constituents of the procedure Itwas found that 05mL of 05Mpotassium iodide solutionwassuitable for PGZ-HCl while 07mL for CRVwas sufficient forthe production of maximum and reproducible color intensity(Figure 6)

314 Effect of Nitric Acid Volume Different volumes of nitricacid were added to a fixed concentration of each drug inthe presence of other constituents of the procedure It wasfound that 07mL of 2 (vv) of nitric acid solution wassuitable for PGZ-HCl while 03mL for CRVwas sufficient forthe production of maximum and reproducible color intensity(Figure 7)

315 Effect of Extracting Solvent Many organic solvents weretried to extract the binary complexes formed Preliminary


Table2Determinationof

PGZ-HCl

andCR

Vthroug

hternarycomplex

form

ationwith

bism

uthtetraiod

ideb

yMetho

dAlowast

PGZ-HCl

CRV

Procedure1

Procedure2

Procedure1

Procedure2

Con

cTaken120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

5488

9753

151520

1013

110

987

9872

161604

10028

1099

49941

252499

9994

252512

10048

242413

10055

151501

10004

353492

9976

4040

1010025

403950

9875

252514

10054

4544

92

9981

606016

10027

484781

9960

353527

10076

555534

10061

706952

10032

565612

10021

454503

10007

656513

10019

808022

10028

727193

9990

504974

9947

Mean

9969

10027

9998

9988

plusmnSD

107

059

07

064

plusmnRS

D10

7059

07

064

SE041

024

029

026

Varia

nce

115

035

049

041

Slop

e27642

00143

37383

00136

LOD120583gm

Lminus1

182

266

310

585

LOQ120583gm

Lminus1

553

806

939

1471

Sand

ellrsquos

sensitivity

120583gcmminus2

000

0103

0067

000

0171

0096

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

38301

059

2295

942times103

lowast

Averageo

fthree

different

trialsof

determ

inations


0005

01015

02025

03035

04045

05

0 02 04 06 08 1Volume of bismuth subnitrate (mL)

Abso

rban

ce (m

AU)

Pioglitazone-HClCarvedilol

Figure 5 Effect of volume of 33 times 10minus3M bismuth subnitrateon the ion pair formed with (i) 20 120583gmLminus1 PGZ-HCl and 05mL05M potassium iodide and (ii) 40120583gmLminus1 CRV and 07mL 05Mpotassium iodide

01

015

02

025

03

035

04

045

05

01 03 05 07 09 11Volume of KI (mL)

Abso

rban

ce (m

AU)


Figure 6 Effect of volume of 05M Potassium iodide on the ionpair formed with (i) 20120583gmLminus1 PGZ-HCl and 03mL 33 times 10minus3Mbismuth subnitrate and (ii) 40 120583gmLminus1 CRV and 04mL 33times10minus3Mbismuth subnitrate

experiments with number of organic solvents commonlyused such as methylene chloride ethyl acetate ethylenechloride benzene and petroleum ether were constructedIt was found that methylene chloride was the appropriatesolvent for the studied drugs

316 Effect of Addition Order The sequence of additionof the constituents of the complex was studied The mostsuitable order was bismuth subnitrate potassium iodidedrug and then nitric acid to give most stability with highersensitivity complex

317 Effect of Reaction and Shaking Times Maximum colorintensity was attained immediately for CRV while PGZ-HClneeded 5 minutes and complete extraction was attained by

02

025

03

035

04

045

05

0 05 1 15Volume of 2 nitric acid (mL)

Abso

rban

ce (m

AU)


Figure 7 Effect of volume of 2 nitric acid on the ion pair formedwith (i) 20120583gmLminus1 PGZ-HCl and (ii) 40 120583gmLminus1 CRV

0

005

01

015

02

025

03

035

04

0 20 40 60Reaction time (min)

Abso

rban

ce (m

AU)


Figure 8 Stability of the ion pair formed between bismuth tetraio-dide and both (i) 10 120583gmLminus1 PGZ-HCl and (ii) 24 120583gmLminus1 CRV

shaking for 1 minute for PGZ-HCl and 2 minutes for CRVThe intensities of the color produced were found to be stablefor more than 1 hour (Figure 8)

318 Composition of the Ion Pair The composition of the ionpairs formed was studied by Jobrsquos method of nonequimolarsolutions [45] Bismuth subnitrate molecule contains fiveatoms of bismuth so upon reaction with potassium iodide itgives fivemolecules of bismuth tetraiodide complex after thatthe formed complex interacts with the studied drugs whichcontain one site for the interaction and gives the ion pair inthe ratio (5 1) but this is difficult practically nonequimolarsolutionsmethod is used for determination of themolar ratioof the formed ion pair The obtained results showed that


0

02

04

06

08

1

12

0 05 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)

Figure 9 Continuous variation plot for PGZ-HCl (13 times 10minus3M)and CRV (13 times 10minus3M) with bismuth subnitrate (26 times 10minus4M)

the composition of the ion pairs was (1 1) for both drugs(Figure 9)

Method Validation The method was validated according tothe International Conference of Harmonization (ICH) [46]

(1) Linearity and Concentration Ranges

For Procedure 1 Graph of the absorbance against concentra-tions proved to be linear in the range from 5 to 50 120583gmLminus1for PGZ-HCl and from 10 to 80 120583gmLminus1 for CRV anddetermination coefficients (1198772) were 09999 for both drugs


(2) Limits of Detection and Limits of Quantitation

For Procedure 1 Limit of detection (LOD) was found to be182 and 310 120583gmLminus1 for PGZ-HCl and CRV respectivelyLimit of quantitation (LOQ)was found to be 553120583gmLminus1 and993 120583gmLminus1 for PGZ-HCl and CRV respectively

For Procedure 2 Limit of detection (LOD) was found to be266 and 558 120583gmLminus1 for PGZ-HCl and CRV respectivelyLimit of quantitation (LOQ) was found to be 806120583gmLminus1and 1471 120583gmLminus1 for PGZ-HCl andCRV respectively Resultsare given in Table 2

(3) Specificity of the Method Results of the analysis werecompared statistically to a reported method for PGZ-HCland CRV applying the Studentrsquos 119905-test and the varianceratio test (119865-test) The results gave lower values than thetheoretical ones indicating no significant difference between

1000

0500

0000

minus020040000 50000 60000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)

Figure 10 Absorption spectra of (a) the reaction of 3 120583gmLminus1 PGZ-HCl with 1mL fast green FCF(001 wv) (b) 1mL fast greenFCF(001 wv) against methylene chloride and (c) 3 120583gmLminus1PGZ-HCl against methylene chloride

1000

0500

0000

minus020050000 55000 60000 65000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)

Figure 11 Absorption spectra of (a) the reaction of 25 120583gmLminus1CRV with 1mL fast green FCF (001 wv) (b) 1mL fast greenFCF(001 wv) against methylene chloride and (c) 25 120583gmLminus1CRV against methylene chloride

the performance of the proposed method and the reportedmethods (Table 3)

(4) Repeatability and Precision of the Method Table 4 showsthat there are high intra- and interday precision Intradayprecision was assessed by injection of the standard solutionof the drug at three concentration levels six times during adayThe same was done for interday precision test except thatthe experiment was done and the drugs were analyzed everyday for six days

32 Reaction with Organic Dyes (Method B)

321 Fast Green FCF Method Absorption spectra of thereagents with PGZ-HCl and CRV were studied over range of200ndash800 nm

Fast green FCF reacts with PGZ-HCl and CRV to yielda blue colored complex exhibitingmaximum absorption at631 nm (Figures 10 and 11) and the ion pair formed can


Table 3 Statistical analysis of results obtained byMethodA applied onDiabetin tablets and Carvid tablets compared with referencemethods

ParametersProcedure 1 Procedure 2 Procedure 1 Procedure 2

Diabetintablets

Referencemethod [12]

Diabetintablets


Carvidtablets


Carvidtablets


119873 4 8 5 8 5 8 5 8Meanrecovery 10077 10023 10074 10023 10088 10002 9935 10002

Variance 112 085 066 085 080 064 029 064plusmnSD 106 092 081 092 089 080 053 080plusmnRSD 111 092 080 092 088 080 053 080plusmnSE 053 033 036 033 040 028 024 028Studentrsquos119905-test

0914(223)a

101(220)a

181(220)a

164(220)a

119865-test 132(435)b

129(412)b

125(412)b

221(412)b

a and b are the theoretical student 119905-values and 119865-ratios at 119875 = 005

Table 4 Evaluation of the interday and intraday precision and accuracy for PGZ-HCl and CRV through Method A

DrugTakenconc(120583gmLminus1)

Interday IntradayRecovery()a

Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

10 9965 076 minus035 10093 119 09315 10084 092 084 10057 103 05740 10019 053 019 10022 089 022

CRV15 9957 116 minus043 9917 078 minus08324 9998 078 minus002 9981 121 minus01950 9906 095 minus094 10085 145 085

RSD percentage relative standard deviationEr percentage relative erroraMean of five trials of determination

be extracted with methylene chloride Different variablesaffecting the reaction were studied

(1) Effect of pH on the Ion-Pair Formations In order to estab-lish the optimum pH value for each ion pair formed variousacids for example acetic hydrochloric and sulphuric acidsof different molarities were studied The highest absorbancevalues were obtained using 01M hydrochloric acid and001M acetic acid for PGZ-HCl and CRV respectively Theoptimum volume used for CRV was 04mL of 001M aceticacid to give the highest absorbance values while 01Mhydrochloric acid was used as solvent for PGZ-HCl and foracidification of the medium (Figure 12)

(2) Effect of Reagent Conc and Volume as well as AdditionsOrder The effect of reagent concentration was also studiedHighest constant absorbance was obtained on using 1mL offast green FCF (001 wv) for both drugs PGZ-HCl andCRV (Figure 13) Moreover the sequence of addition of theconstituents of the complex was also studied Addition of thedrug followed by the dye and then the acidwas recommendedto obtain stable high color intensity

(3) Choice of Organic Solvent A solvent is needed to extractthe formed ion-pair to increase the selectivity of the assay

071072073074075076077078079

08081

008 018 028 038 048Volume of acetic acid (mL)

Abso

rban

ce (m

AU)

Carvedilol

Figure 12 Effect of HAc volume on the ion-pair complex formationbetween 001 wv fast green FCF and 25120583gmLminus1 CRV

Preliminary experiment with a number of organic solventscommonly used (benzene ethylacetate methylene chlorideand ethylene chloride) for the ion-pair extraction was stud-ied Methylene chloride was the appropriate solvent because


Table 5 Analytical parameters for the determination of PGZ-HCl and CRV via Method B

Parameters PGZ-HCl CRVFast green FCF Orange G Fast green FCF Orange G

Conc of reagent wv 001 04 001 02Vol of reagent mL 1 05 1 05120582max nm 631 498 631 498Beerrsquos law limits 120583gmLminus1 05ndash4 10ndash70 05ndash3 5ndash45Regression equationlowast

Intercept 01116 minus00413 minus00055 00168Slope 01945 00143 03201 00206Correlation Coefficient 09999 09999 09999 09999Molar Ratio 2 3 1 1 1 1 1 1

lowast

119860 = 119886 + 119887119862 where 119862 is the concentration of drug in 120583gmLminus1 119860 is the absorbance 119886 is the intercept and 119887 is the slope

02025

03035

04045

05055

06065

0 05 1Volume of fast green dye (mL)

Abso

rban

ce (m

AU)


Figure 13 Effect of volume of 001 wv fast green FCF dye onthe ion-pair complex formation with 25 120583gmLminus1 PGZ-HCl and1 120583gmLminus1 CRV respectively

of its higher sensitivity and lower extraction ability of thereagents

(4) Effect of Reaction Time and Number of Extraction TimesReaction time required for complete color development ofion-pair complexes formed between the studied drugs andfast green FCF was studied Maximum color intensity wasattained immediately for both drugs to reach its maximumintensity Complete extraction was attained by double extrac-tion with (2 times 5mL) methylene chloride and then completeto 10mL with the same solvent The intensities of the colorproducedwere found to be stable for about 1 hr for both drugs(Figure 14)

(5) Composition of the Ion-Pair Complexes The compositionof the ion pairwas studied by Jobrsquosmethod of continuous vari-ation [44]The obtained results showed that the compositionof ion pair complexes was (1 1) (drug reagent) for PGZ-HCland (2 3) (drug reagent) for CRV (Figure 15)

0

01

02

03

04

05

06


Abso

rban

ce (m

AU)


Figure 14 Stability of the ion pair formed between fast green FCFand both (i) 05 120583gmLminus1 PGZ-HCl and (ii) 15 120583gmLminus1 CRV

322 Orange GMethod Absorption spectra of the reagentswith PGZ-HCl and CRV were studied over range of 200ndash800 nm Orange G reacts with PGZ-HCl and CRV to yield anorange colored chromophore exhibitingmaximum absorp-tion at 498 nm (Figures 16 and 17) and the ion pair formedcan be extracted with methylene chloride

Different Variables Affecting the Reaction Were Studied

(1) Effect of pH on the Ion-Pair Formation In order to establishthe optimum pH value for each ion pair formed variousacids like hydrochloric sulphuric and acetic acids of differentmolarities were studied The highest absorbance values wereobtained using 05M sulphuric acid and 2M acetic acid forPGZ-HCl and CRV respectively

The optimum volume used for CRV was 02mL of 2Macetic acid to give the highest absorbance values while 05Msulphuric acid was used as solvent for PGZ-HCl and foracidification of the medium (Figure 18)

(2) Choice of Organic Solvents The results using differentextracting solvents (benzene ethylacetate methylene chlo-ride and ethylene chloride) indicated thatmethylene chloride


0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)

Figure 15 Continuous variation plot for PGZ-HCl (1times10minus4M) andCRV (1 times 10minus4M) with fast green FCF (1 times 10minus4M)

1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)

Figure 16 Absorption spectra of (a) the reaction of 60 120583gmLminus1PGZ-HCl with 05mL orange G (04 wv) against methylenechloride (b) 05mL orange G (04 wv) against methylenechloride and (c) 60 120583gmLminus1 PGZ-HCl against methylene chloride

is the most appropriate solvent for extraction and that can beattributed to its high extraction efficiency

(3) Effect of Reagent Conc and Volume as well as AdditionsOrder The effect of reagent concentration was also studiedHighest constant absorbance was obtained on using 05mL of(04 wv) and (02 wv) orange G for PGZ-HCl and CRVrespectively (Figure 19) Moreover the sequence of additionof the constituents of the complex was also studied Additionof the drug followed by the dye and then the acid wasrecommended to obtain stable high color intensity

(4) Effect of Reaction Time and Number of Extraction TimesReaction time required for complete color developmentof ion-pair complexes formed between the studied drugsand orange G was studied Maximum color intensity wasattained immediately for both drugs Complete extractionwas attained by double extraction with (2 times 5mL) methylenechloride and then complete to 10mL with the same solventThe intensities of the color produced were found to be stablefor about 1 hr for both drugs (Figure 20)

1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)

Figure 17 Absorption spectra of (a) the reaction of 40 120583gmLminus1CRV with 05mL orange G (02 wv) (b) 05mL orange G (02wv) against methylene chloride and (c) 40 120583gmLminus1 CRV againstmethylene chloride

Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol

Figure 18 Effect of HAc volume on the ion-pair complex formationbetween 02 wv orange G and 25 120583gmLminus1 CRV

(5) Composition of the Ion-Pair ComplexThe composition ofthe ion-pair was studied by Jobrsquos method of continuous vari-ation [44] The obtained results showed that the compositionof ion-pair complex was (3 2) (drug reagent) for PGZ-HCland (1 1) (drug reagent) for CRV (Figure 21)



Fast Green FCF Method Graph of the absorbance againstconcentrations proved to be linear in the range from 05 to4 120583gmLminus1 for PGZ-HCl and from 05 to 3 120583gmLminus1 for CRVand determination coefficients (1198772) were 09999 for bothdrugs (Table 5)

Orange GMethod Graph of the absorbance against con-centrations proved to be linear in the range from 10 to70 120583gmLminus1 for PGZ-HCl and from 5 to 45 120583gmLminus1 for CRV


03035

04045

05055

06065

07

0 05 1 15 2Volume of orange G dye

Abso

rban

ce (m

AU)


Figure 19 Effect of volume of 04 wv and 02 wv orange G dye on the ion-pair complex formation with 50 120583gmLminus1 PGZ-HCl and25 120583gmLminus1 CRV respectively

0

01

02

03

04

05

06

0 20 40 60 80Reaction time (min)

Abso

rban

ce (m

AU)


Figure 20 Stability of the ion pair formed between orange G andboth (i) 10120583gmLminus1 PGZ-HCl and (ii) 25 120583gmLminus1 CRV

and determination coefficients (1198772) were 09999 for bothdrugs (Table 5)


Fast Green FCF Method Limit of detection (LOD) wasfound to be 013 and 0078 120583gmLminus1 for PGZ-HCl and CRVrespectively Limit of quantitation (LOQ) was found tobe 039 120583gmLminus1 and 024120583gmLminus1 for PGZ-HCl and CRVrespectively

Orange GMethod Limit of detection (LOD) was found to be023 and 016 120583gmLminus1 for PGZ-HCl and CRV respectivelyLimit of quantitation (LOQ) was found to be 07120583gmLminus1 and049 120583gmLminus1 for PGZ-HCl and CRV respectively Results aregiven in Table 6


0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s

Figure 21 Continuous variation plot for PGZ-HCl (2times10minus3M)withorange G (2 times 10minus3M) and CRV (7 times 10minus4M) with orange G (7 times10minus4M)



4 Conclusions

The two proposed methods for determination of PGZ andCRV are based on the formation of ion-pair associates


Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination


Table 7 Statistical analysis of results obtained byMethod B applied on Diabetin tablets and Carvid tablets compared with reported methods

ParametersDiabetin tablets Carvid tablets

Fast greenFCF Orange G

Referencemethod[12]

Fast greenFCF Orange G Reference

method [13]

119873 4 5 8 5 5 8Mean recovery 10021 10041 10023 10018 10026 10002Variance 051 050 085 038 028 064plusmnSD 072 071 092 062 053 080plusmnRSD 072 071 092 062 053 080plusmnSE 036 032 033 028 024 028

Studentrsquos 119905-test 0038(223)a

041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b


Table 8 Evaluation of the interday and intraday precision and accuracy for PGZ-HCl and CRV obtained by Method B

Drug MethodTakenconc(120583gmLminus1)


Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen

1 9894 180 minus106 9924 103 minus0762 9955 109 minus045 9997 095 minus0033 10013 078 013 9865 117 minus135

Orange G10 9941 131 minus059 9871 119 minus12930 10145 098 145 9989 117 minus01160 9908 113 minus092 10165 096 165

CRV

Fastgreen

1 9888 121 minus112 9856 123 minus1442 10176 086 176 9987 138 minus0133 9968 149 minus032 9878 117 minus122

Orange G10 10043 131 043 10057 114 05725 9813 087 minus187 10167 126 16740 9987 134 minus013 10199 087 199


between the drugs and the inorganic complex bismuth(III)tetraiodide (Method A) and between the drugs and theorganic acidic dyes fast green and orangeG (MethodB) Bothmethods were found to be sensitive accurate and preciseWhen the results obtained by the proposed methods werecompared with those of reference methods there was nosignificant differenceTheproposedmethodswere applied fordetermination of the analytes in drug dosage form with goodaccuracy and without interference

Conflict of Interests

The authors declare that there is no conflict of interestsregarding the publication of this paper

References

[1] S C SweetmanMartindale the Complete Drug Reference 36thedition 2009

[2] M Chennaiah T Veeraiah T C Singh andG VenkateshwarluldquoExtractive spectrophotometric methods for determination ofPGZ using acidic triphenylmethane dyesrdquo Asian Journal ofResearch in Chemistry vol 4 no 6 pp 971ndash975 2011

[3] Z H Qin G M Shen Y S Liu and H S Luo ldquoSpectropho-tometric method for determination of PGZ with eosin YrdquoQinzonghui Fenxi Shiyanshi vol 27 no 10 pp 15ndash18 2008

[4] R S Mehta D M Patel K K Bhatt and M B ShankarldquoUV and visible spectrophotometric analysis of pioglitazonehydrochloride in bulk and tabletsrdquo Indian Journal of Pharma-ceutical Sciences vol 67 no 4 pp 487ndash489 2005


[5] K Sujana K Abbulu O Bala Souri B Archana M Sinduand G Swathi Rani ldquoDifference spectrophotometric methodsfor pioglitazone hydrochloride and metform in hydrochloriderdquoJournal of Pharmaceutical Sciences and Research vol 3 no 4pp 1122ndash1126 2011

[6] S Sharma and M C Sharma ldquoDetermination of atorvastatincalcium and pioglitazone HCl in pharmaceutical formulationsform by using atomic absorption spectrometryrdquoOptoelectronicsand Advanced Materials Rapid Communications vol 4 no 8pp 1196ndash1199 2010

[7] N A Al-Arfaj E A Al-Abdulkareem and F A Aly ldquoFlow-injection chemiluminometric determination of pioglitazoneHCl by its sensitizing effect on the cerium-sulfite reactionrdquoAnalytical Sciences vol 25 no 3 pp 401ndash406 2009

[8] N A Al-Arfaj E A Al-Abdulkareem and F A Aly ldquoAvalidated adsorptive stripping voltammetric determination ofantidiabetic agent pioglitazone HCl in tablets and biologicalfluidsrdquo International Journal of Biomedical Science vol 4 no 4pp 310ndash318 2008

[9] A A Abdelmonem G H Ragab H Hashem and E A BahgatldquoHigh performance liquid chromatographic and spectrophoto-metric determinations of PGZ-HCl either alone or in combina-tion with Metformin-HClrdquo Journal of Liquid Chromatographyamp Related Technologies vol 35 pp 2706ndash2723 2012

[10] A Shirkhedkar and S Surana ldquoApplication of a stability-indicating densitometric RP-TLCmethod for analysis of piogli-tazone hydrochloride in the bulk material and in pharmaceu-tical formulationsrdquo Journal of Planar Chromatography ModernTLC vol 22 no 3 pp 191ndash196 2009

[11] B Siddartha and B Sudheer ldquoAnalytical method developmentand method validation for the estimation of PGZ in tabletdosage form by RP-HPLCrdquo International Journal of Pharmacyand Pharmaceutical Sciences vol 5 no 3 pp 770ndash774 2013

[12] P K Basniwal P K Srivastava and D Jain ldquoSpectrophotomet-ric estimation of PGZ in tablet dosage formrdquo Asian Journal ofPharmaceutical vol 2 pp 225ndash227 2008

[13] N Verma A K Ghosh and P Chattopadhyay ldquoSimultaneousspectrophotometric determination of CRV in its dosage formrdquoInternational Journal of Pharma Sciences and Research vol 1 no12 pp 188ndash190 2010

[14] The British Pharmacopoeia Volumes II and III Her MajestyrsquosStationery Office London UK 2009

[15] S G Cardoso C V S Ieggli and S C G Pomblum ldquoSpec-trophotometric determination of carvedilol in pharmaceuticalformulations through charge-transfer and ion-pair complexa-tion reactionsrdquo Pharmazie vol 62 no 1 pp 34ndash37 2007

[16] C Theivarasu S Ghosh and T Indumathi ldquoUV spectropho-tometric determination of carvedilol in pharmaceutical formu-lationsrdquo Asian Journal of Pharmaceutical and Clinical Researchvol 3 no 4 pp 64ndash68 2010

[17] Y N Rani B V Ravikumar and S Mohanty ldquoDevelopmentand validation of new analytical methods for the estimationof carvedilol in bulk and pharmaceutical dosage formsrdquo AsianJournal of Pharmaceutical and Clinical Research vol 6 no 2 pp138ndash140 2013

[18] S D Manohar D A Sridhar and S C Mallikarjuna ldquoDevel-opment of UV spectrophotometric method for estimation ofcarvedilol in bulk and pharmaceutical formulationsrdquo AsianJournal of Research in Chemistry vol 6 no 10 pp 956ndash9592013

[19] I Leonenko D Aleksandrova and A Yegorova ldquoDetermina-tion of carvedilol by its quenching effect on the luminescence of

terbiumcomplex in dosage formrdquoActa Poloniae PharmaceuticaDrug Research vol 68 no 3 pp 325ndash330 2011

[20] A Onal ldquoSpectrophotometric and spectrofluorimetric deter-mination of some drugs containing secondary amino group inbulk drug and dosage forms via derivatization with 7-chloro-4-nitrobenzofurazonrdquo Quımica Nova vol 34 no 4 pp 677ndash6822011

[21] C V S Ieggli S G Cardoso and L P Belle ldquoValidation of UVspectrophotometric and nonaqueous titration methods for thedetermination of carvedilol in pharmaceutical formulationsrdquoJournal of AOAC International vol 88 no 5 pp 1299ndash13032005

[22] R S Haggag R A Shaalan and T S Belal ldquoValidated HPLCdetermination of the two fixed dose combinations (chlor-diazepoxide hydrochloride and mebeverine hydrochloridecarvedilol and hydrochlorothiazide) in their tabletsrdquo Journal ofAOAC International vol 93 no 4 pp 1192ndash1200 2010

[23] P Sripalakit S Kaewnok and S Tubtonglang ldquoDevelopmentof carvedilol assay in tablet dosage form using HPLC withfluorescence detectionrdquo Maejo International Journal of Scienceand Technology vol 4 no 1 pp 8ndash19 2010

[24] J Stojanovi S Vladimirov V Marinkovi D Velikovi and PSibinovi ldquoMonitoring of the photochemical stability of CRVand its degradation products by the RP-HPLCmethodrdquo Journalof the Serbian Chemical Society vol 72 pp 37ndash44 2007

[25] M Sylwia A Weronika and B Irena ldquoSimultaneous chiralseparation and determination of CRV and 51015840-hydroxyphenylCRV enantiomers from human urine by high performanceliquid chromatography coupled with fluorescent detectionrdquoCentral European Journal of Chemistry vol 11 no 12 pp 2076ndash2087 2013

[26] T S Belal F A El Yazbi R A Shaalan and S MElonsy ldquoValidated stability-indicating HPLC-DAD determina-tion of the antihypertensive binary mixture of carvedilol andhydrochlorothiazide in tablet dosage formsrdquo Chromatographiavol 76 no 23-24 pp 1707ndash1720 2013

[27] D P Patel P Sharma M Sanyal P Singhal and P S ShrivastavldquoUPLC-MSMS assay for the simultaneous quantification ofcarvedilol and its activemetabolite 4rsquo-hydroxyphenyl carvedilolin human plasma to support a bioequivalence study in healthyvolunteersrdquo Biomedical Chromatography vol 27 no 8 pp 974ndash986 2013

[28] F M Abdel-Gawad ldquoIon-pair formation of Bi(III)-iodide withsome nitrogenous drugs and its application to pharmaceuticalpreparationsrdquo Journal of Pharmaceutical and Biomedical Analy-sis vol 16 no 5 pp 793ndash799 1998

[29] L M Abdellaziz and M M Hosny ldquoDevelopment and vali-dation of spectrophotometric atomic absorption and kineticmethods for determination of moxifloxacin hydrochloriderdquoAnalytical Chemistry Insights vol 6 no 1 pp 67ndash78 2011

[30] A M El-Brashy M E-S Metwally and F A El-Sepai ldquoSpec-trophotometric and atomic absorption spectroscopic deter-mination of some fluoroquinolone antibacterials by ion-paircomplex formation with bismuth (III) tetraiodiderdquo Journal ofthe Chinese Chemical Society vol 52 no 2 pp 253ndash262 2005

[31] MAyadHAbdellatefMHosny andNKabil ldquoConductomet-ric determination of certain pharmacological drugs using silverand bismuthrdquo International Research Journal of Pharmaceuticaland Applied Sciences vol 3 no 4 pp 140ndash148 2013

[32] C S P Sastry M Aruna M Narayana Reddy and D GSankar ldquoExtractive spectrophotometric determination of some


anthelmintics using fast green FCF or orange-IIrdquo Indian Journalof Pharmaceutical Sciences vol 50 no 2 pp 140ndash142 1988

[33] K Sreedhar C S P Sastry M Narayana Reddy and DG Sankar ldquoSpectrophotometric determination of mebeverinehydrochloriderdquoMikrochimica Acta vol 126 no 1-2 pp 131ndash1351997

[34] M Kishore K Surendrababu C S R G Kalyani and MJanardhan ldquoSpectrophotometric determination of ceftiofur inpharmaceutical formulations by FGFCF SFNO and MBrdquo Jour-nal of Pharmaceutical Sciences and Research vol 2 no 9 pp534ndash538 2010

[35] LQiu-hua ldquoKinetic spectrophotometric determination of traceruthenium with fast green FCFrdquo Chinese Journal of AnalysisLaboratory vol 26 pp 60ndash62 2007

[36] J Zhiliang and Q Qin Chen-zhen ldquoA new application of fastgreen in catalytic analysis-catalytic determination of ultratraceruthenium with oscillopolarographic detectionrdquo Electroanaly-sis vol 5 pp 535ndash537 1993

[37] S Pillai and I Singhvi ldquoApplication of orange G dye for quan-titation of citalopram hydrobromide donepezil hydrochlorideand rabeprazole sodium from tablet formulationrdquo Indian Jour-nal of Pharmaceutical Sciences vol 68 no 5 pp 682ndash684 2006

[38] A Bhandage A Bhosale A Kasture and V P Godse ldquoExtrac-tive spectrophotometric determination of omeprazole in phar-maceutical preparationsrdquo Tropical Journal of PharmaceuticalResearch vol 8 no 5 pp 449ndash454 2009

[39] B Rajitha S Prashanthi K Ramsubha Reddy and G TuljaRani ldquoExtractive spectrophotometric determination of tra-madol hydrochloride in pure and pharmaceutical dosageformsrdquo International Journal of PharmTech Research vol 3 no1 pp 114ndash117 2011

[40] R Tulja Rani D Gowri Sankar P Kadgapathi R Suthakaranand B Satyanarayana ldquoVisible spectrophotometric methodsfor the determination of drotaverine hydrochloride in bulkand in pharmaceutical formulationsrdquo International Journal ofPharmTech Research vol 2 no 3 pp 1787ndash1791 2010

[41] H M Saleh M M EL-Henawee G H Ragab and S S AbdEL-Hay ldquoExtractive spectrophotometric determination of someantihistaminic and skeletal muscle relaxant drugs through ion-pair formation with xylene cyanol and orange Grdquo Bulletin ofFaculty of Pharmacy Cairo University vol 45 no 3 pp 373ndash3902007

[42] G Jie Y Ming-Hui Y Zhi-Yi L Zu-Bi and C Qiu-E ldquoKineticspectrophotometric determination of trace ruthenium withorangeGrdquoChinese Journal of Analysis Laboratory vol 2 pp 38ndash40 2005

[43] S Motomizu M Oshima and Y Hosoi ldquoSpectrophotometricdetermination of cationic and anionic surfactants with anionicdyes in the presence of nonionic surfactants part I a generalaspectrdquoMikrochimica Acta vol 106 no 1-2 pp 57ndash66 1992

[44] J Mendham R C Denney J D Barnes andMThomasVogelrsquosTextbook of Quantitative Chemical Analysis Pearson EducationEssex UK 2000

[45] W C Vosburg andG R Cooper ldquoJobmethod of non equimolarsolutionrdquo Journal of the American Chemical Society vol 63 pp437ndash442 1941

[46] ldquoGuidance for Industry Q2B of Analytical ProceduresMethodololgy International Conference of Harmonization(ICH)rdquo 1996

Submit your manuscripts athttpwwwhindawicom

Hindawi Publishing Corporationhttpwwwhindawicom Volume 2014

Inorganic ChemistryInternational Journal of

Hindawi Publishing Corporation httpwwwhindawicom Volume 2014

International Journal ofPhotoenergy


Carbohydrate Chemistry

International Journal of


Journal of

Chemistry


Advances in

Physical Chemistry

Hindawi Publishing Corporationhttpwwwhindawicom

Analytical Methods in Chemistry

Journal of

Volume 2014

Bioinorganic Chemistry and ApplicationsHindawi Publishing Corporationhttpwwwhindawicom Volume 2014

SpectroscopyInternational Journal of


The Scientific World JournalHindawi Publishing Corporation httpwwwhindawicom Volume 2014

Medicinal ChemistryInternational Journal of


Chromatography Research International


Applied ChemistryJournal of



Theoretical ChemistryJournal of


Journal of

Spectroscopy

Analytical ChemistryInternational Journal of


Journal of


Quantum Chemistry


Organic Chemistry International

ElectrochemistryInternational Journal of



CatalystsJournal of


O

N

NH

S

O

O

middotHCl

H3C

(a)

OO

NH

HN

H OH

OCH3

And enantiomer

(b)

Figure 1 Chemical structures of (a) PGZ-HCl and (b) CRV

indicated for the treatment of hypertension angina pectorisand heart failure [1]

CRV and its pharmaceutical formulations have beenassayed in BP [14] which describes nonaqueous titrationby dissolving the drug in anhydrous acetic acid and thentitration with 01M perchloric acid determining the end-point potentiometrically Several spectrophotometric meth-ods have been reported for estimation of CRV includingion-pair complex formation with bromocresol green andbromothymol blue as well as charge-transfer reaction ofthe drug with the sigma-acceptor iodine [15] Also UVspectrophotometric determination ofCRV inpharmaceuticalformulations was applied [16ndash18] Other methods includingdetermination of CRV by its quenching effect on the lumi-nescence of terbium complex in dosage form [19] spectroflu-orimetric determination via derivatization with 7-Chloro-4-niritrobenzofurazon [20] and nonaqueous titration [21]have been described Chromatographic methods have beenreported such as validated HPLC determination of the fixeddose combination (CRV and hydrochlorothiazide) in theirtablets [22] HPLC with fluorescence detection [23] and RP-HPLC method for monitoring of the photochemical stabilityof CRV and its degradation products [24] A Chiral HPLC-separation and determination of CRV from human urine wasalso noticed [25] A stability-indicating HPLC-DAD deter-mination of a mixture of carvedilol and hydrochlorothiazide[26] and also UPLC-MSMS method for assay of carvediloland its active metabolite in human plasma were introduced[27] No atomic absorption spectrometricmethods have beenpreviously reported for CRV determination

Bismuth(III)-iodide compounds have been used asreagents for determination of some nitrogenous drugs suchas amineptine hydrochloride piribedil and trimebutinemaleate [28] It has been also used for spectrophotomet-ric and atomic absorption spectroscopic determination ofmoxifloxacin hydrochloride [29] as well as levofloxacinnorfloxacin and ciprofloxacin [30] It has been also usedfor conductometric determination of lomefloxacine HClpantoprazole sodium and sumatriptan succinate [31] Onmixing aqueous solutions of bismuth(III) tetraiodide com-plex and the cited drugs in an acidic medium a reddishorange precipitate instantaneously appeared that is attributedto the ion pair formed in the reaction (Scheme 1)The formedprecipitates are then extracted and quantified spectrophoto-metrically at 490 nm or filtered dried and then decomposed

by hydrochloric acid and the bismuth content is determinedby AAS at 2231 nm [31]

Fast green FCF (Figure 2(a)) is an acidic dye used forspectrophotometric determination of some anthelmintics[32] mebeverine [33] and ceftiofur [34] It has been also usedfor kinetic spectrophotometric determination of trace ruthe-nium [35] and in catalytic analysis of ultratrace rutheniumwith oscillopolarographic detection [36]

OrangeG (Figure 2(b)) is also an acidic dye used for spec-trophotometric determination of citalopram hydrobromidedonepezil hydrochloride rabeprazole sodium [37] fromtablet formulation omeprazole [38] tramadol hydrochloride[39] drotaverine hydrochloride [40] and some antihis-taminic and skeletal muscle relaxant drugs [41] It has beenalso used for spectrophotometric determination of traceruthenium [42] and cationic and anionic surfactants in thepresence of nonionic surfactants [43]

In this paper new and simple atomic absorption spec-troscopic and spectrophotometric methods are proposed fordetermination of some nitrogenous drugs based on theformation of ion pair associated with Bi(III)-iodide complexfast green or orangeG dyesThe proposedmethods have beenapplied to the assay of these drugs in tablets

2 Experiment

21 Apparatus All of the spectrophotometric measurementswere carried out using a Shimadzu UV-1800 with matched1 cm quartz cells (Japan) A Lutron digital pH-meter was usedfor pH adjustment (103 Taipei Taiwan) Shimadzu atomicabsorption spectrophotometric model AA-640-13 was used

22 Materials All solutions were prepared with analytical-grade chemicals and water was always doubly distilled Thestudied drugs were of pharmaceutical grade Standard bis-muth(III) solution 33 times 10minus3M was prepared by dissolving04824 g of bismuth subnitrate (Evans united kingdom) in5mL of conc HNO

3

and adding distilled water and stan-dardized complexometrically [43] 05M potassium iodidewas prepared by dissolving 833 g of KI (Universal finechemicals PVT-LTD India) in 100mL of water Solutions oflower concentration were obtained by accurate dilution ofthese solutions with water Acetic acid hydrochloric acidand sulphuric acid solutions of different molarities wereprepared as in recommended methods [44] Fast green FCF


ONH

S

O

ON

ONH

S

O

ONH

NH

O NH

O

OH

OMe

NH

O

OH

NO

OMe

HH

minus

+

Pioglitazone


Carvedilol


H+

H+

H3C

H3C

+

+

+

Bi(I)4

minus

Bi(I)4

minus

Bi(I)4

minus

Bi(I)4


OH

SO3minus

SO3minus

minusO3S

N

N+

(a)

OH

NN

SO3Na

SO3Na

(b)











amount of 05MH2

SO4





For Method A



3



2

H2





3


For Method B








For Method B



2

SO4




For Method B












lowastlowast


(a)

(b)

(c)

1000

0500

0000

minus0100

Abso

rban

ce (m

AU)

39999 45000 50000 55000

(nm)



3




(a)

(b)

(c)

1000

0800

0600

0400

0200

000040000 45000 50000 55000

(nm)

Abso

rban

ce (m

AU)







PGZ-HCl

andCR

Vthroug

hternarycomplex

form

ationwith

bism

uthtetraiod

ideb

yMetho

dAlowast

PGZ-HCl

CRV

Procedure1

Procedure2

Procedure1

Procedure2

Con

cTaken120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

5488

9753

151520

1013

110

987

9872

161604

10028

1099

49941

252499

9994

252512

10048

242413

10055

151501

10004

353492

9976

4040

1010025

403950

9875

252514

10054

4544

92

9981

606016

10027

484781

9960

353527

10076

555534

10061

706952

10032

565612

10021

454503

10007

656513

10019

808022

10028

727193

9990

504974

9947

Mean

9969

10027

9998

9988

plusmnSD

107

059

07

064

plusmnRS

D10

7059

07

064

SE041

024

029

026

Varia

nce

115

035

049

041

Slop

e27642

00143

37383

00136

LOD120583gm

Lminus1

182

266

310

585

LOQ120583gm

Lminus1

553

806

939

1471

Sand

ellrsquos

sensitivity

120583gcmminus2

000

0103

0067

000

0171

0096

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

38301

059

2295

942times103

lowast

Averageo

fthree

different

trialsof

determ

inations


0005

01015

02025

03035

04045

05


Abso

rban

ce (m

AU)



01

015

02

025

03

035

04

045

05

01 03 05 07 09 11Volume of KI (mL)

Abso

rban

ce (m

AU)






02

025

03

035

04

045

05


Abso

rban

ce (m

AU)



0

005

01

015

02

025

03

035

04


Abso

rban

ce (m

AU)






0

02

04

06

08

1

12

0 05 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)











1000

0500

0000

minus020040000 50000 60000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


1000

0500

0000

minus020050000 55000 60000 65000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)










Diabetintablets


Diabetintablets


Carvidtablets


Carvidtablets


119873 4 8 5 8 5 8 5 8Meanrecovery 10077 10023 10074 10023 10088 10002 9935 10002


0914(223)a

101(220)a

181(220)a

164(220)a

119865-test 132(435)b

129(412)b

125(412)b

221(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

10 9965 076 minus035 10093 119 09315 10084 092 084 10057 103 05740 10019 053 019 10022 089 022







071072073074075076077078079

08081


Abso

rban

ce (m

AU)

Carvedilol








lowast


02025

03035

04045

05055

06065


Abso

rban

ce (m

AU)






0

01

02

03

04

05

06


Abso

rban

ce (m

AU)









0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)


1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)





1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol








03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of


ONH

S

O

ON

ONH

S

O

ONH

NH

O NH

O

OH

OMe

NH

O

OH

NO

OMe

HH

minus

+

Pioglitazone


Carvedilol


H+

H+

H3C

H3C

+

+

+

Bi(I)4

minus

Bi(I)4

minus

Bi(I)4

minus

Bi(I)4


OH

SO3minus

SO3minus

minusO3S

N

N+

(a)

OH

NN

SO3Na

SO3Na

(b)











amount of 05MH2

SO4





For Method A



3



2

H2





3


For Method B








For Method B



2

SO4




For Method B












lowastlowast


(a)

(b)

(c)

1000

0500

0000

minus0100

Abso

rban

ce (m

AU)

39999 45000 50000 55000

(nm)



3




(a)

(b)

(c)

1000

0800

0600

0400

0200

000040000 45000 50000 55000

(nm)

Abso

rban

ce (m

AU)







PGZ-HCl

andCR

Vthroug

hternarycomplex

form

ationwith

bism

uthtetraiod

ideb

yMetho

dAlowast

PGZ-HCl

CRV

Procedure1

Procedure2

Procedure1

Procedure2

Con

cTaken120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

5488

9753

151520

1013

110

987

9872

161604

10028

1099

49941

252499

9994

252512

10048

242413

10055

151501

10004

353492

9976

4040

1010025

403950

9875

252514

10054

4544

92

9981

606016

10027

484781

9960

353527

10076

555534

10061

706952

10032

565612

10021

454503

10007

656513

10019

808022

10028

727193

9990

504974

9947

Mean

9969

10027

9998

9988

plusmnSD

107

059

07

064

plusmnRS

D10

7059

07

064

SE041

024

029

026

Varia

nce

115

035

049

041

Slop

e27642

00143

37383

00136

LOD120583gm

Lminus1

182

266

310

585

LOQ120583gm

Lminus1

553

806

939

1471

Sand

ellrsquos

sensitivity

120583gcmminus2

000

0103

0067

000

0171

0096

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

38301

059

2295

942times103

lowast

Averageo

fthree

different

trialsof

determ

inations


0005

01015

02025

03035

04045

05


Abso

rban

ce (m

AU)



01

015

02

025

03

035

04

045

05

01 03 05 07 09 11Volume of KI (mL)

Abso

rban

ce (m

AU)






02

025

03

035

04

045

05


Abso

rban

ce (m

AU)



0

005

01

015

02

025

03

035

04


Abso

rban

ce (m

AU)






0

02

04

06

08

1

12

0 05 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)











1000

0500

0000

minus020040000 50000 60000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


1000

0500

0000

minus020050000 55000 60000 65000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)










Diabetintablets


Diabetintablets


Carvidtablets


Carvidtablets


119873 4 8 5 8 5 8 5 8Meanrecovery 10077 10023 10074 10023 10088 10002 9935 10002


0914(223)a

101(220)a

181(220)a

164(220)a

119865-test 132(435)b

129(412)b

125(412)b

221(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

10 9965 076 minus035 10093 119 09315 10084 092 084 10057 103 05740 10019 053 019 10022 089 022







071072073074075076077078079

08081


Abso

rban

ce (m

AU)

Carvedilol








lowast


02025

03035

04045

05055

06065


Abso

rban

ce (m

AU)






0

01

02

03

04

05

06


Abso

rban

ce (m

AU)









0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)


1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)





1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol








03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of










amount of 05MH2

SO4





For Method A



3



2

H2





3


For Method B








For Method B



2

SO4




For Method B












lowastlowast


(a)

(b)

(c)

1000

0500

0000

minus0100

Abso

rban

ce (m

AU)

39999 45000 50000 55000

(nm)



3




(a)

(b)

(c)

1000

0800

0600

0400

0200

000040000 45000 50000 55000

(nm)

Abso

rban

ce (m

AU)







PGZ-HCl

andCR

Vthroug

hternarycomplex

form

ationwith

bism

uthtetraiod

ideb

yMetho

dAlowast

PGZ-HCl

CRV

Procedure1

Procedure2

Procedure1

Procedure2

Con

cTaken120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

5488

9753

151520

1013

110

987

9872

161604

10028

1099

49941

252499

9994

252512

10048

242413

10055

151501

10004

353492

9976

4040

1010025

403950

9875

252514

10054

4544

92

9981

606016

10027

484781

9960

353527

10076

555534

10061

706952

10032

565612

10021

454503

10007

656513

10019

808022

10028

727193

9990

504974

9947

Mean

9969

10027

9998

9988

plusmnSD

107

059

07

064

plusmnRS

D10

7059

07

064

SE041

024

029

026

Varia

nce

115

035

049

041

Slop

e27642

00143

37383

00136

LOD120583gm

Lminus1

182

266

310

585

LOQ120583gm

Lminus1

553

806

939

1471

Sand

ellrsquos

sensitivity

120583gcmminus2

000

0103

0067

000

0171

0096

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

38301

059

2295

942times103

lowast

Averageo

fthree

different

trialsof

determ

inations


0005

01015

02025

03035

04045

05


Abso

rban

ce (m

AU)



01

015

02

025

03

035

04

045

05

01 03 05 07 09 11Volume of KI (mL)

Abso

rban

ce (m

AU)






02

025

03

035

04

045

05


Abso

rban

ce (m

AU)



0

005

01

015

02

025

03

035

04


Abso

rban

ce (m

AU)






0

02

04

06

08

1

12

0 05 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)











1000

0500

0000

minus020040000 50000 60000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


1000

0500

0000

minus020050000 55000 60000 65000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)










Diabetintablets


Diabetintablets


Carvidtablets


Carvidtablets


119873 4 8 5 8 5 8 5 8Meanrecovery 10077 10023 10074 10023 10088 10002 9935 10002


0914(223)a

101(220)a

181(220)a

164(220)a

119865-test 132(435)b

129(412)b

125(412)b

221(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

10 9965 076 minus035 10093 119 09315 10084 092 084 10057 103 05740 10019 053 019 10022 089 022







071072073074075076077078079

08081


Abso

rban

ce (m

AU)

Carvedilol








lowast


02025

03035

04045

05055

06065


Abso

rban

ce (m

AU)






0

01

02

03

04

05

06


Abso

rban

ce (m

AU)









0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)


1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)





1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol








03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of







For Method B



2

SO4




For Method B












lowastlowast


(a)

(b)

(c)

1000

0500

0000

minus0100

Abso

rban

ce (m

AU)

39999 45000 50000 55000

(nm)



3




(a)

(b)

(c)

1000

0800

0600

0400

0200

000040000 45000 50000 55000

(nm)

Abso

rban

ce (m

AU)







PGZ-HCl

andCR

Vthroug

hternarycomplex

form

ationwith

bism

uthtetraiod

ideb

yMetho

dAlowast

PGZ-HCl

CRV

Procedure1

Procedure2

Procedure1

Procedure2

Con

cTaken120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

5488

9753

151520

1013

110

987

9872

161604

10028

1099

49941

252499

9994

252512

10048

242413

10055

151501

10004

353492

9976

4040

1010025

403950

9875

252514

10054

4544

92

9981

606016

10027

484781

9960

353527

10076

555534

10061

706952

10032

565612

10021

454503

10007

656513

10019

808022

10028

727193

9990

504974

9947

Mean

9969

10027

9998

9988

plusmnSD

107

059

07

064

plusmnRS

D10

7059

07

064

SE041

024

029

026

Varia

nce

115

035

049

041

Slop

e27642

00143

37383

00136

LOD120583gm

Lminus1

182

266

310

585

LOQ120583gm

Lminus1

553

806

939

1471

Sand

ellrsquos

sensitivity

120583gcmminus2

000

0103

0067

000

0171

0096

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

38301

059

2295

942times103

lowast

Averageo

fthree

different

trialsof

determ

inations


0005

01015

02025

03035

04045

05


Abso

rban

ce (m

AU)



01

015

02

025

03

035

04

045

05

01 03 05 07 09 11Volume of KI (mL)

Abso

rban

ce (m

AU)






02

025

03

035

04

045

05


Abso

rban

ce (m

AU)



0

005

01

015

02

025

03

035

04


Abso

rban

ce (m

AU)






0

02

04

06

08

1

12

0 05 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)











1000

0500

0000

minus020040000 50000 60000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


1000

0500

0000

minus020050000 55000 60000 65000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)










Diabetintablets


Diabetintablets


Carvidtablets


Carvidtablets


119873 4 8 5 8 5 8 5 8Meanrecovery 10077 10023 10074 10023 10088 10002 9935 10002


0914(223)a

101(220)a

181(220)a

164(220)a

119865-test 132(435)b

129(412)b

125(412)b

221(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

10 9965 076 minus035 10093 119 09315 10084 092 084 10057 103 05740 10019 053 019 10022 089 022







071072073074075076077078079

08081


Abso

rban

ce (m

AU)

Carvedilol








lowast


02025

03035

04045

05055

06065


Abso

rban

ce (m

AU)






0

01

02

03

04

05

06


Abso

rban

ce (m

AU)









0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)


1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)





1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol








03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of






lowastlowast


(a)

(b)

(c)

1000

0500

0000

minus0100

Abso

rban

ce (m

AU)

39999 45000 50000 55000

(nm)



3




(a)

(b)

(c)

1000

0800

0600

0400

0200

000040000 45000 50000 55000

(nm)

Abso

rban

ce (m

AU)







PGZ-HCl

andCR

Vthroug

hternarycomplex

form

ationwith

bism

uthtetraiod

ideb

yMetho

dAlowast

PGZ-HCl

CRV

Procedure1

Procedure2

Procedure1

Procedure2

Con

cTaken120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

5488

9753

151520

1013

110

987

9872

161604

10028

1099

49941

252499

9994

252512

10048

242413

10055

151501

10004

353492

9976

4040

1010025

403950

9875

252514

10054

4544

92

9981

606016

10027

484781

9960

353527

10076

555534

10061

706952

10032

565612

10021

454503

10007

656513

10019

808022

10028

727193

9990

504974

9947

Mean

9969

10027

9998

9988

plusmnSD

107

059

07

064

plusmnRS

D10

7059

07

064

SE041

024

029

026

Varia

nce

115

035

049

041

Slop

e27642

00143

37383

00136

LOD120583gm

Lminus1

182

266

310

585

LOQ120583gm

Lminus1

553

806

939

1471

Sand

ellrsquos

sensitivity

120583gcmminus2

000

0103

0067

000

0171

0096

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

38301

059

2295

942times103

lowast

Averageo

fthree

different

trialsof

determ

inations


0005

01015

02025

03035

04045

05


Abso

rban

ce (m

AU)



01

015

02

025

03

035

04

045

05

01 03 05 07 09 11Volume of KI (mL)

Abso

rban

ce (m

AU)






02

025

03

035

04

045

05


Abso

rban

ce (m

AU)



0

005

01

015

02

025

03

035

04


Abso

rban

ce (m

AU)






0

02

04

06

08

1

12

0 05 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)











1000

0500

0000

minus020040000 50000 60000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


1000

0500

0000

minus020050000 55000 60000 65000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)










Diabetintablets


Diabetintablets


Carvidtablets


Carvidtablets


119873 4 8 5 8 5 8 5 8Meanrecovery 10077 10023 10074 10023 10088 10002 9935 10002


0914(223)a

101(220)a

181(220)a

164(220)a

119865-test 132(435)b

129(412)b

125(412)b

221(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

10 9965 076 minus035 10093 119 09315 10084 092 084 10057 103 05740 10019 053 019 10022 089 022







071072073074075076077078079

08081


Abso

rban

ce (m

AU)

Carvedilol








lowast


02025

03035

04045

05055

06065


Abso

rban

ce (m

AU)






0

01

02

03

04

05

06


Abso

rban

ce (m

AU)









0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)


1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)





1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol








03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of



PGZ-HCl

andCR

Vthroug

hternarycomplex

form

ationwith

bism

uthtetraiod

ideb

yMetho

dAlowast

PGZ-HCl

CRV

Procedure1

Procedure2

Procedure1

Procedure2

Con

cTaken120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

Con

cTaken

120583gm

Lminus1

Con

cFo

und

120583gm

Lminus1

Recovery

()

5488

9753

151520

1013

110

987

9872

161604

10028

1099

49941

252499

9994

252512

10048

242413

10055

151501

10004

353492

9976

4040

1010025

403950

9875

252514

10054

4544

92

9981

606016

10027

484781

9960

353527

10076

555534

10061

706952

10032

565612

10021

454503

10007

656513

10019

808022

10028

727193

9990

504974

9947

Mean

9969

10027

9998

9988

plusmnSD

107

059

07

064

plusmnRS

D10

7059

07

064

SE041

024

029

026

Varia

nce

115

035

049

041

Slop

e27642

00143

37383

00136

LOD120583gm

Lminus1

182

266

310

585

LOQ120583gm

Lminus1

553

806

939

1471

Sand

ellrsquos

sensitivity

120583gcmminus2

000

0103

0067

000

0171

0096

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

38301

059

2295

942times103

lowast

Averageo

fthree

different

trialsof

determ

inations


0005

01015

02025

03035

04045

05


Abso

rban

ce (m

AU)



01

015

02

025

03

035

04

045

05

01 03 05 07 09 11Volume of KI (mL)

Abso

rban

ce (m

AU)






02

025

03

035

04

045

05


Abso

rban

ce (m

AU)



0

005

01

015

02

025

03

035

04


Abso

rban

ce (m

AU)






0

02

04

06

08

1

12

0 05 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)











1000

0500

0000

minus020040000 50000 60000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


1000

0500

0000

minus020050000 55000 60000 65000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)










Diabetintablets


Diabetintablets


Carvidtablets


Carvidtablets


119873 4 8 5 8 5 8 5 8Meanrecovery 10077 10023 10074 10023 10088 10002 9935 10002


0914(223)a

101(220)a

181(220)a

164(220)a

119865-test 132(435)b

129(412)b

125(412)b

221(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

10 9965 076 minus035 10093 119 09315 10084 092 084 10057 103 05740 10019 053 019 10022 089 022







071072073074075076077078079

08081


Abso

rban

ce (m

AU)

Carvedilol








lowast


02025

03035

04045

05055

06065


Abso

rban

ce (m

AU)






0

01

02

03

04

05

06


Abso

rban

ce (m

AU)









0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)


1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)





1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol








03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of


0005

01015

02025

03035

04045

05


Abso

rban

ce (m

AU)



01

015

02

025

03

035

04

045

05

01 03 05 07 09 11Volume of KI (mL)

Abso

rban

ce (m

AU)






02

025

03

035

04

045

05


Abso

rban

ce (m

AU)



0

005

01

015

02

025

03

035

04


Abso

rban

ce (m

AU)






0

02

04

06

08

1

12

0 05 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)











1000

0500

0000

minus020040000 50000 60000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


1000

0500

0000

minus020050000 55000 60000 65000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)










Diabetintablets


Diabetintablets


Carvidtablets


Carvidtablets


119873 4 8 5 8 5 8 5 8Meanrecovery 10077 10023 10074 10023 10088 10002 9935 10002


0914(223)a

101(220)a

181(220)a

164(220)a

119865-test 132(435)b

129(412)b

125(412)b

221(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

10 9965 076 minus035 10093 119 09315 10084 092 084 10057 103 05740 10019 053 019 10022 089 022







071072073074075076077078079

08081


Abso

rban

ce (m

AU)

Carvedilol








lowast


02025

03035

04045

05055

06065


Abso

rban

ce (m

AU)






0

01

02

03

04

05

06


Abso

rban

ce (m

AU)









0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)


1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)





1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol








03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of


0

02

04

06

08

1

12

0 05 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)











1000

0500

0000

minus020040000 50000 60000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


1000

0500

0000

minus020050000 55000 60000 65000 70000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)










Diabetintablets


Diabetintablets


Carvidtablets


Carvidtablets


119873 4 8 5 8 5 8 5 8Meanrecovery 10077 10023 10074 10023 10088 10002 9935 10002


0914(223)a

101(220)a

181(220)a

164(220)a

119865-test 132(435)b

129(412)b

125(412)b

221(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

10 9965 076 minus035 10093 119 09315 10084 092 084 10057 103 05740 10019 053 019 10022 089 022







071072073074075076077078079

08081


Abso

rban

ce (m

AU)

Carvedilol








lowast


02025

03035

04045

05055

06065


Abso

rban

ce (m

AU)






0

01

02

03

04

05

06


Abso

rban

ce (m

AU)









0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)


1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)





1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol








03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of




Diabetintablets


Diabetintablets


Carvidtablets


Carvidtablets


119873 4 8 5 8 5 8 5 8Meanrecovery 10077 10023 10074 10023 10088 10002 9935 10002


0914(223)a

101(220)a

181(220)a

164(220)a

119865-test 132(435)b

129(412)b

125(412)b

221(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

10 9965 076 minus035 10093 119 09315 10084 092 084 10057 103 05740 10019 053 019 10022 089 022







071072073074075076077078079

08081


Abso

rban

ce (m

AU)

Carvedilol








lowast


02025

03035

04045

05055

06065


Abso

rban

ce (m

AU)






0

01

02

03

04

05

06


Abso

rban

ce (m

AU)









0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)


1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)





1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol








03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of






lowast


02025

03035

04045

05055

06065


Abso

rban

ce (m

AU)






0

01

02

03

04

05

06


Abso

rban

ce (m

AU)









0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)


1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)





1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol








03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of


0

01

02

03

04

05

06

07

08

0 02 04 06 08 1

Abso

rban

ce (m

AU)


Vd (Vd + Vr)


1000

0500

0000

minus020040000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)





1000

0500

0000

minus020042000 45000 50000 55000 60000

(nm)

(a)

(b)(c)

Abso

rban

ce (m

AU)


Carvedilol

035

04

045

05

055


Abso

rban

ce (m

AU)

Carvedilol








03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of


03035

04045

05055

06065

07


Abso

rban

ce (m

AU)



0

01

02

03

04

05

06


Abso

rban

ce (m

AU)








0

01

02

03

04

05

06

07

08

Abso

rban

ce (m

AU)

0 05 1


Vd (Vd + Vr)

s




4 Conclusions



Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of


Table6Re

sults

ofthea

nalysis

ford

eterminationof

PGZ-HCl

andCR

V(authentic)u

singMetho

dB

Parameters

PGZ-HCllowast

CRVlowast

FastgreenFC

Fmetho

dOrang

eGmetho

dFastgreenFC

Fmetho

dOrang

eGmetho

dTaken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

Taken

120583gm

Lminus1

Foun

d120583gm

Lminus1

Recovery

05

051

10118

101002

10021

05

050

9966

5501

10019

1099

9943

202002

10010

110

09950

101001

10010

1515

110057

302981

9937

1515

010007

201986

9932

219

89907

403995

9988

2201

10036

252525

1010

125

251

10024

505044

10088

25

251

10041

303011

10036

3300

9998

606023

10038

3299

9960

4040

01

10002

4400

10005

706974

9963

454506

10013

Mean

10008

10007

9993

10016

plusmnSD

070

050

040

050

plusmnRS

D070

050

040

050

plusmnSE

026

019

016

019

Varia

nce

049

025

016

025

Slop

e01945

00143

03201

00206

LOD120583gm

Lminus1

013

023

0078

016

LOQ120583gm

Lminus1

039

07

024

049

Sand

ellrsquos

sensitivity

120583gcmminus2

00036

0078

00032

004

6

Apparent

Molar

absorptiv

ityLM

olminus1 cmminus1

1087times104

050times104

1283times104

088times104

lowast

Averageo

fthree

different

trialsof

determ

ination





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of





Referencemethod[12]


method [13]



041(220)a

133(220)a

059(220)a

119865-test 167(435)b

170(412)b

167(412)b

227(412)b





Precision(RSD)a

Accuracy(Er)

Recovery()a

Precision(RSD)a

Accuracy(Er)

PGZ-HCl

Fastgreen



CRV

Fastgreen







References




























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of
























































Journal of

Chemistry


Advances in

Physical Chemistry



Journal of

Volume 2014














Journal of

Spectroscopy



Journal of


Quantum Chemistry






CatalystsJournal of

research article simple atomic absorption spectroscopic...

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