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SAMPLE

Matrix: blood

Sample preparat ion:

Condition a Bond-Elut C18 SPE cartridge with M eOH and water.

Add

500 |xL

plasma

to the SPE

cartridge, wash with

2 mL

water, wa sh with

2 mL

MeO H: water 20:80 , elute w ith

two 500

|JLL aliquots

of

MeOH. Evaporate

the

eluate

to

dryness under a stream of nitrogen, reconstitute the residue in 50 |xL MeOH : water 20:

80,

inject a 20 JULL aliquot.

HPLCVARIABLES

Column:

100 X 1 5 |xm Hyp ersil ODS

Mobile phase:

MeCN : MeO H: water 25:25 :50

Flow rate: 0.1

Inject ion vo lum e:

20

Detector: UV

CHROMATOGRAM

Retent ion t ime:

20

Limit of detect ion:

2

ng/mL

OTHER SUBSTANCES

Extracted:

androstenedione, 20a-hydroxy-4-pregnen-3-one, 17a-hydroxyprogesterone, pro-

gesterone, testosterone

KEYWORDS

microbore; rat; plasma; SPE

REFERENCE

Taylor,

R.B.;

Kendle,

K.E.;

Reid,

R.G.;

Hung,

CT.

Chromatography

of

progesterone

and its

major

me-

tabolites

in rat

plasma using microbore high-performance liquid chromatography columns with

con-

ventional injection

and

detection systems. J.Chromatogr.,

1987, 385,

383—392

SAMPLE

Matrix:

blood


2 mL

Plasma

5 mL

hexan e: dichloromethane

1:1,

shake

for 10 min,

centrifuge at 2000 rpm for 10 min. Remove 4 mL of the organic phas e and evaporate it at

55° under nitrogen. Reconstitute residue in 300 |xL mobile p has e, inject a 150 |xL aliquot.

HPLCVARIABLES

Column:

250 X 4.6 5 |xm

L iChrosorb

RP-8

Mobile phase:

MeO H: MeCN : water 20:30 :50

Flow rate: 2

Inject ion volume:

150

Detector:

UV 254

CHROMATOGRAM

Retent ion t ime: 8

Limit

of

qu ant i ta t ion:

2

ng/mL

Norethindrone

Molecular formu la: G

20

H

26

O

2

Molecular weight:

298.4

CAS Registry No :

68-22 -4, 51-98-9 acetate)


2/9

KEYWORDS

plasma

REFERENCE

Loo,

J.C.K.;

Brien,

R.

Analysis

of

norethindrone

in

plasma

by

high-performance liquid chromatography.

J.Liq.Chromatogr. 1981

4

871-877

SAMPLE

Matrix: bulk

HPLCVARIABLES

Column:

250 X 4 10 jxin LiChrosorb RP-18

Mobile phase: MeOH: water 70:30

Flow rate: 1

Injection volume: 25

Detector: UV 240

CHROMATOGRAM

Retent ion t ime: 7

OTHER SUBSTANCES

Simultaneous:

ethinyl estradiol, impurities, norgestrel

REFERENCE

Gdrdg, S.; Herenyi, B. Analysis of stero ids . XXXVIIL The use of high-performance liquid chrom atography

with diode-array

UV

detection

for

estimating impurity profiles

of

steroid d rugs. J.Chromatogr.

1987

400

177-186

SAMPLE

Matrix: food

Sample preparation:

Dissolve apple extracts in THF, inject a 10 |xL extract.

HPLCVARIABLES

Column:

300 X 3.9 jxBondapak C18

Mobile phase: MeOH: THF: water 11:26:63

Flow rate: 1.7


Detector: UV

254

CHROMATOGRAM

Retention time: 11.6

OTHER SUBSTANCES

Simultaneous:

degradation products, impurities

KEYWORDS

apples; fruit; stability-indicating

REFERENCE

Mayberry, D.O.; Kow blansky, M.; L ane, RA.; Wray, RE. Determination of norethindrone stability on Red

Delicious apples. J.Pharm.ScL

1990

79 746-749

SAMPLE

Matrix: formulations


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Sample p re par at io n : Dissolve 12 tablets in 600 mL water with stirring at 75 rpm, remove

3 mL sample, centrifuge at 3000 rpm for 15 min, inject a 250 |xL aliquot.

HPLCVARIABLES

Colu mn: 100 X 4.6 3 jxm Phenomenex IB-SiI 3 C18

Mobile p ha se : MeCN: water 40:60, pH 5.6

Flow rate: 1.2


D etec tor: UV 200

C H R O M A T O G R A M

Retention time: 7.7

OTHER SUBSTANCES

Simultaneous: ethinyl estradiol

KEYWORDS

tablets; modification of USP method

REFERENCE

Dorantes, A.; Stavchansky, S. Modification of the U.S.P. dissolution method for the analysis of noreth-

indrone and ethinyl estradiol tablets. J.Pharm.ScL 1994, 83 3 7 9 - 3 8 1

SAMPLE


Sam ple p re pa ra tion : Dissolve 6 tablets in 600 mL water: isopropanol 97:3, remove 5 mL

samples, centrifuge at 1500 rpm for 10 min, inject a 50-200 |xL aliquot.

HPLCVARIABLES

Column: 300 X 3.9 10 jxm Bondapak C18

M obile ph as e: MeCN: water 55:45

Flow rate: 1

Injection volume: 50-200

Detec tor: UV 200

OTHER SUBSTANCES

Simultaneous: mestranol

KEYWORDS

tablets; modified USP method

REFERENCE

Nguyen, H.T.; Shiu, G.K.; Worsley, W.N.; Skelly, J.R Dissolution testing of norethindrone: ethinyl estra-

diol, n orethindrone : mestranol, and norethindrone ace tate: ethinyl estradiol combination tablets.

J.Pharm.ScL 1990 79 163-167

SAMPLE


Sa m ple p re para ti on : Dissolve 6 tablets in 600 mL 100 mM HCl containing 0.02 sodium

lauryl sulfate, remove 5 mL samples, centrifuge at 1500 rpm for 10 min, inject a 50-200

IxL aliquot.

HPLCVARIABLES

Colu mn: 220 X 4.6 5 |jim Spheri-5 C18

Mobile p has e: MeCN: 20 mM pH 6.0 phosphate buffer 35:65


4/9


5/9


10

Detector:

U V 240

CHROMATOGRAM

Retent ion t ime:

4.6 (norethindrone), 8.6 (norethindrone acetone)

Limit of detect ion: 5 jig/mL

OTHER SUBSTANCES

Simul taneous:

asp irin, benzyl alcohol, benzyl ben zoate, caffeine, calu stero ne, cortisone, de-

hydroepiandrosterone (UV 210), formebolone, mesterolone (UV 210), methandriol (UV

210), m ethandrostenolone, m ethenolone acetate, methyltestosterone, m ibolerone, nandro-

lone, nandrolone acetate, nandrolone propionate, norethandrolone, norgestrel, oxymeth-

olone, stanozolol, testolactone, testostero ne, testostero ne a cetate, testos terone propion ate,

trenbolone acetate

Interfering:

boldenone, ethisterone, fluoxymesterone, oxandrolone (UV 210)

KEYWORDS

oils;

tablets; suspensions

REFERENCE

Walters, M.J.; Ayers, R.J.; Brown, D.J. Analysis of illegally distributed anabolic steroid products by

liquid chromatography with identity confirmation by mass spectrometry or infrared spectrophotom-

etry J.Assoc.Off.Anal.Chem. 1990 73 904-926

SAMPLE

Matrix:

formulations


Dissolve 5 g cream con taining 0.00925 fluocinonide, 0.00365 pro-

cinonide, and 0.0021 ciprocinonide in 2.5 mL THF, add norethin dron e, dilute to 25 mL

with MeOH, centrifuge, inject a 25 JULL aliquot onto column A with mobile ph ase A and

allow com ponents to elu te from column A to column B for 7 m in. After 7 m in rem ove

column A from circuit, mo nitor effluent from column B . Back-flush column A w ith m obile

pha se B for 5 min, equ ilibrate column A with mobile ph ase A for 5 min before next

injection.

HPLCVARIABLES

Column: A 30 X 4.6 5 >jim Spheri-5 ODS (B rownlee); B 70 X 2.1 Wh atm an Co :Pell ODS +

250 X 4.6 5 |jim U ltras ph ere C18

Mobile phase: A M eCN :THF:water 4 3:4 :53 ; B MeOH :THF 75:25

Flow rate: A 1.5; B 1

Inject ion volume:

25

Detector:

UV 260 for 22 min then UV 236

CHROMATOGRAM

Retent ion t ime: 12

Internal s tandard: norethindrone

OTHER SUBSTANCES

Simul taneous: ciprocinonide, fluocinolone acetonide, fluocinonide, procinonide

KEYWORDS

creams; column-switching; norethindrone is IS

REFERENCE

Conley, D.L.; Benjamin, E.J. Automated high-performance liquid chromatographic column switching

techniqu e for the on-line clean-up and analy sis of drugs in topical cream formulations. J.Chromatogr.

1983, 257 337-344


6/9

SAMPLE



1 Tablet + 4 mL 50 mM KH

2

PO

4

, rotate 15 min, add 2 mL 1 ixg/mL

o-phenylphenol in mobile pha se, add 4 mL MeOH , rot ate 15 min , centrifuge. Remove

supernatant, extract residue twice with 5 mL mobile phase (10 min rotation), combine

supernatants, inject 50

|JLL

aliquot.

HPLC VARIABLES

Column: 250 X 4.6 10 (xm L iChrosorb RP 8

M obile pha se: MeOH:50 mM KH

2

PO

4

3:2

Flow rate: 2

Inject ion volum e: 50

De tecto r: UV 220

CHROMATOGRAM

Retent ion t ime:

9 (norethindrone), 19.3 (norethindrone acetate)

OTHER SUBSTANCES

Simul taneous:

methyltestosterone, norgestrel

Interfering: ethinyl estradiol

KEYWORDS

tablets; stability-indicating

REFERENCE

Strus iak, S.H.; Hoogerheide, J.G.; G ardner, M.S. Determ ination of ethinyl estrad iol in solid dosage forms

by high-performance liquid chromatography.

J.Pharm.Sci.

1982

71

636-640

SAMPLE

Matrix:

reaction mixtures

Sample preparat ion: If necessary, remove oxidizing power of solution by adding sodium

metabisulfite, inject a 20

JJLL

aliquot.

HPLC VARIABLES

Guard column: 15 X 4.6 5 |xm M icrosorb C8

Column:

250 X 4.6 5 |xm Microsorb C8

Mobile phase:

M eCN: 100 mM KH

2

PO

4

adjusted to pH 7 with 1 M KOH 50:5 0

Flow rate: 1

Inject ion volume: 20

Detector: UV

254

CHROMATOGRAM

Retent ion t ime: 8 .7

Limit of detect ion: 100 ng/mL

REFERENCE

L unn , G.; Rhodes, S.W.; Sanso ne, E.B.; Schmuff, N.R. Photolytic destruction and polymeric resin decon-

tamination of aqueous solutions of pharmaceuticals.

J.Pharm.Sci.

1994

83

1289-1293

SAMPLE

Matrix:

solutions

HPLCVARIABLES

Column: 50 X 4.6 5 Jim Supelcosil L C-18

Mobile phase:

MeOH : TH F: water 10:20:70


7/9

Flow rate: 2


Detector: UV 220

CHROMATOGRAM

Retent ion t ime: 3 (norethindrone), 7.4 (norethindrone acetate)

OTHER SUBSTANCES

Simul taneous: ethinyl estradiol, norethynodrel acetate, norgestrel

REFERENCE

Supelco Catalog Supelco Inc Bellefonte PA

1996, p. A130

SAMPLE

Matrix:

solutions

Sample preparat ion: Inject a 5 JJLL aliquo t of a 10 jxg/mL solution in M eOH.

HPLCVARIABLES

Column: 75 X 4.6 3 fxm U ltras ph ere ODS

Mobile phase:

MeC N: 10 mM am mon ium acetate buffer 45:5 5

Flow rate: 0 .5


Detector: UV 254

CHROMATOGRAM

Retent ion t ime:

5.941

OTHER SUBSTANCES

Simul taneous: boldenone, epime thand ienon e, ep itestosterone, fluoxymesterone, 6p-hy-

droxymethandienone, methandienone, oxymetholone (UV 280), trenbolone

REFERENCE

Barron, D.; Pascual, J.A.; Segura, J.; Barbosa, J. Prediction of LC retention of steroids using solvato-

chromic parameters. Chromatographia 1995, 41 573-580

SAMPLE

Matrix: solutions


Inject a 20

\iL

aliquot of a solution in MeO H: w ater 50:5 0.

HPLCVARIABLES

Column:

250 X 4 7 |jim L ichroCAR T RP -8 (Merck)

Mobile phase:

MeCN: MeOH: water 32:37:31

Flow rate: 1


20

Detector: UV

230

CHROMATOGRAM

Retent ion t ime: 5

OTHER SUBSTANCES

Simul taneous: fluoxymesterone, m edrogestone, m estrano l, progesterone, tes tostero ne

propionate


8/9

REFERENCE

Gau, YS.; Sun, S.W.; Chem, R.R.-L. Optimization of high-performance liquid chromatographic separa-

tion for progestogenic, estrogenic, and androgenic steroids usin g factorial design. J.Liq.Chromatogr.

1995, 18 2373-2382

SAMPLE

Matrix: solutions

HPLCVARIABLES

Column: 250 X 4.6 10 ^m Nucleosil C18

Mobile phase: MeCN:THF-.water 12.9:22.4:64.7

Flow rate: 1

D etecto r: UV 240

CHROMATOGRAM

Retent ion t ime:

8.5 (norethindrone), 15.5 (norethindrone acetate)

OTHER SUBSTANCES

Simul taneous:

estrone, ethinyl estradiol, mestranol, norgestrel

REFERENCE

Gazdag, M.; Szepesi, G.; Szeleczki, E. Selection of high-performance liquid chromatographic methods in

pharmaceutical analysis. I. Optimization for selectivity in reversed-phase chromatography.

J.Chromatogr.

1988

454 8 3 - 9 4

SAMPLE

Matrix: solutions

HPLCVARIABLES

Column: 250 X 4.6 5 ^m L iChrosorb Si 60

Mobile phase: Hex ane: dioxane: isopropanol 95 :3: 2

Flow rate: 1

Detector: UV 254

CHROMATOGRAM

Retent ion t ime:

20 (norethindrone), 10 (norethindrone acetate)

OTHER SUBSTANCES

Simul taneous: estrone, ethinyl estradiol, mestranol, norgestrel

KEYWORDS

normal phase

REFERENCE

Gazdag, M .; Szepesi, G.; Fabian-Varga, K. Selection of high-performance liquid chrom atographic m eth-

ods in pharmaceutical analysis. II. Optimization for selectivity in normal-phase systems.

J.Chromatogr.

1988

454 9 5 - 1 0 7

SAMPLE

Matrix: solutions

Sample preparat ion: Dissolve in MeO H: w ate r 1:1 at a conc entration of 50 |xg/mL , inject

a 10

|JLL

aliquot.

HPLCVARIABLES

Column:

300

X 3.9 10 |xm

(xBondapak C18


9/9

Mobile phase:

MeOH: acetic acid: triethylamine: water 60:1.5:0.5:38

FIo

5

W rate: 1.5


Detector: UV 240

CHROMATOGRAM

Retention time: 12

OTHER SUBSTANCES

Simultaneous: hydrocortisone acetate, methyltestosterone, prednisolone, prednisolone suc-

cinate, prednisone, progesterone

REFERENCE

Roos,

R.W.;

L au-Cam,

CA.

Gen eral reversed-ph ase high-performance liquid chromatograp hic method

for

the

separation

of

drugs using triethylamine

as a

competing base.

J.Chromatogr.

1986

370

403-418

• • •

ANNOTATED BIBLIOGRAPHY

Tang, G.P.; Chen, Q.Q. [Column switching H PL C method for determination of in vivo relea se of noreth-

indrone-alpha , beta-poly (3-hydroxypropyl)-DL -asparamide conjugate].

Y ao Hsueh Hsueh Pao

1994

29 301-305

Lee, G.J.-L.; Oyang, M.-H.; Bautista,

J.;

Kushinsky,

S.

Determination

of

ethinylestradiol

and

noreth-

indrone

in a

single specimen

of

plasma

by

autom ated high-performance liquid chromatograp hy

and

subsequent radioimmunoassay.

J.Liq.Chromatogr.

1987 10 2305-2318 [LOD 20-50 pg/mL ]

Papas,

A.N.;

Marchese,

S.M.;

Delaney,

M.F.

Rapid determina tion

of

norethindrone

and

ethinylestradiol

in oral contraceptive tablets

by

reversed-phase liquid chromatography.

LC

Mag.

1985

3

354-358

[tablets; column temp

25;

simultaneous ethinylestradiol; Chem.Abs.,

102,

226114]

Swynnerton, N.R; Fischer, J.B. Determination of ethyny lestradiol and norethindrone in synthetic in-

testinal fluid

and in

timed-release oral formulations.

J.Liq.Chromatogr.

1980

3

1195-1204

[for-

mulations; also ethinylestradiol]

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