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Page 1: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's
Page 2: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

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Page 3: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

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Page 4: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

C184-E045

Gas Chromatograph

The Next Industry StandardNexis GC-2030, Shimadzu's premier gas chromatograph, offers a modern approach to a classic chromatographic technique. Designed with the user in mind, new innovative features, exceptional performance and high-throughout capabilities will elevate your lab to the next level.

Designed with the Analyst in Mind

An advanced interface enables intuitive operation with clear graphics. Shimadzu's latest tool-free

maintenance technology makes daily maintenance easy.

World’s Highest*1 Sensitivity and Reproducibility

Achieves the world’s highest*1 sensitivity on the all of the detectors, such as FID and BID. The advanced

flow controller (AFC) enhances reliability with excellent repeatability.

Exceptional Expandability and Productivity

Nexis GC-2030 can be customized to meet a customers' specific requirements and needs. Options and

functions to use hydrogen carrier gas safely in high-speed analysis maximize analysis productivity.

3

Page 5: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

Information at Your Finger-tipsAnalysts will benefit from the touch panel interface, which features

clear graphics that display information instantly whenever needed.

The user-friendly interface leaves the operator free to focus on

obtaining optimal analytical results.

Main settings controllable via the touch panel on the GC unit:

• Analytical conditions• Self-diagnostics• Automatic carrier gas leak check• Chromatogram display, etc.

Tool-free Column InstallationClickTek connectors*2 make tool free column installation a snap.

The click sensation felt when finished attaching the column

provides a more reliable connection and ensures a better seal

under all operating conditions.

*2 Optional

ClickTek Connector

One Touch Inlet Maintenance The injection port can be opened or closed without tools by simply

sliding the ClickTek lever. Replace the insert, slide the lever and feel

the click for a leak-free install every time.

ClickTek Nut

High-Sensitivity Detectors Support a Wide Variety of Analyses

The jet and collector structure on the flame ionization detector

(FID-2030) has been optimized to provide improved performance.

Noise levels were also decreased by improving the stability of the

signal processor and flow controller. This results in the world's most*1

sensitive FID. This makes the Nexis GC-2030 the best choice to

measure residual solvents in pharmaceuticals.

1

2

3

4

5

0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 min

1. 1,1-Dichloroethane2. 1,1,1-Trichloroethane3. Carbontetrachloride4. Benzene5. 1,2-Dichloroethane

Analysis of Trace Residual Solvents in PharmaceuticalsUsing Headspace GC, Class 1 Standard Solution

GC Systems Customized for Specific NeedsThe Nexis GC-2030 provides powerful support for configuring custom

GC systems tailored to user needs. These systems are adjusted and

tested at the factory for the given application before shipment, so

they are ready to use for measurements as soon as they are delivered.

That means no time is required for developing methods after the

system arrives. Two TCD detectors and one FID detector can be

installed at the same time. An optional valve box can be added to

control up to eight valves from the original four.

Examples of System GC Configurations

Gasoline analysis system

This system is able to measure specific substances in gasoline, such as oxygenates.

Natural gas analysis system

This system is able to analyze components in natural gas, such as shale gas.

Inorganic gasanalysis system

This system is able to measure hydrogen and various other inorganic gases.

Hydrocarbonanalysis system

This system is able to measure hydrocarbons that are generated, such as from catalyst reactions.

Refinery gas analysis system

This system is able to analyze components in gas from petroleum refineries.

Public utility natural gas analysis system

This system is able to calculate calorific values from measurements of natural gas.

*1 As of May 2017, according to a Shimadzu survey

© Shimadzu Corporation, 2017

For Research Use Only. Not for use in diagnostic procedures. This publication may contain references to products that are not available in your country. Please contact us to check the availability of these products in your country.Company names, product/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation or its affiliates, whether or not they are used with trademark symbol “TM” or “®”. Third-party trademarks and trade names may be used in this publication to refer to either the entities or their products/services. Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own.

The contents of this publication are provided to you “as is” without warranty of any kind, and are subject to change without notice. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication.www.shimadzu.com/an/

First Edition: May 2017, Printed in Japan 3655-05713-30ANS4

Page 6: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

1 Introduction

The HS-GC-FID method is used to test for residual solvents in pharmaceuticals, but GC-MS is useful for identifying peaks in close

proximity or for qualifying unknown peaks. However, to qualify peaks detected by GC-FID using GC-MS requires matching

chromatogram patterns. The advanced flow controller (AFC) in GC-2010 Plus systems includes constant linear velocity control as

standard functionality. This allows achieving similar retention time and separation patterns in GC-FID and GC-MS chromatograms by

specifying the same linear velocity setting, provided the columns are identical or columns with the same phase ratio are used.

2 Analytical Conditions to Test for Residual Solvents in Pharmaceuticals

Testing for residual solvents in pharmaceuticals involves using a separation column with a 0.53 mm (or 0.32 mm) internal diameter,

30 m length, and 3.0 µm (or 1.8 µm) thick cyanopropyl phenyl-based liquid phase and separation conditions with a linear carrier gas

speed of 35 cm/sec (Procedure A). However, those separation conditions cannot be achieved using GC-MS, due to the negative

pressure (vacuum) at the column outlet. Therefore, the typical method used to obtain similar chromatogram patterns is to downsize

the column to one with a small internal diameter, so that the phase ratio (ratio of column internal diameter to film thickness) is the

same.

Control by the AFC takes into consideration the difference in column outlet pressure between GC and GC-MS. For HS-GCMS analysis,

it simply requires changing the column and specifying a 35 cm/sec linear velocity in the method parameter selection window in

GCMSsolution. During analysis, the AFC controls the carrier gas automatically, which eliminates the inconvenience of having to

adjust pressure or other settings.

GCMS-QP2020 + HS-20 + FID-2010 Plus DetectorBy including an FID detector in the HS-GCMS system, either

analytical method can be used. Contact a Shimadzu representative

regarding changing the system configuration, which can be

modified to accommodate various user requirements.

Using GCMS to Testfor Residual Solvents in Pharmaceuticals

C146-E338

This results in similar chromatogram patternsusing the same linear velocity of 35 cm/sec.

SH Rxi-624sil MS0.32 mm I.D., 30 m long, and 1.8 µmfilm thickness

SH Rxi-624sil MS0.25 mm I.D., 30 m long, and 1.4 µmfilm thickness

5

Page 7: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

3 Comparison of GC-FID and GC-MS Chromatograms

After using a GC-FID system to acquire data from a Class 2 standard solution A, data were acquired using a GC-MS system with the

same linear velocity condition (35 cm/sec). Then the resulting chromatograms were compared. The comparison shows that the shift

in retention times between FID and MS data was 0.02 minutes (1.2 seconds) for acetonitrile, which elutes early, and for cumene,

which elutes late. In addition, both chromatograms were similar, with approximately the same separation patterns.

The GC-MS data showed a peak at roughly the same retention time as for the unknown peak detected by the GC-FID system. This

peak can be identified easily by qualitative analysis, such as by displaying the mass spectrum and using an MS spectral library to

search for a similar peak pattern.

4 Summary

If a HS-GC-MS system is used for qualitative analysis in testing for residual solvents in pharmaceuticals, it is important that the

chromatogram pattern obtained is similar to the chromatogram obtained from HS-GC-FID analysis. The constant linear velocity

control mode for the AFC unit included in Shimadzu GC-MS systems can be used in combination with a Shimadzu HS-20 headspace

sampler. Even if the different-sized columns are used for HS-GC-FID and HS-GC-MS analysis, chromatograms with similar retention

times and separation patterns can be obtained easily by using columns with the same phase ratio and by specifying the same linear

velocity setting, which means GC-MS data can easily be used for qualitative analysis.

© Shimadzu Corporation, 2017

www.shimadzu.com/an/

For Research Use Only. Not for use in diagnostic procedures. This publication may contain references to products that are not available in your country. Please contact us to check the availability of these products in your country.Company names, products/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation, its subsidiaries or its affiliates, whether or not they are used with trademark symbol “TM” or “®”.Third-party trademarks and trade names may be used in this publication to refer to either the entities or their products/services, whether or not they are used with trademark symbol “TM” or “®”.Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own.

The contents of this publication are provided to you “as is” without warranty of any kind, and are subject to change without notice. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication.

Printed in Japan 3655-02707-20AIT

Acetonitrile(4.05 min)

Acetonitrile(4.07 min)

Cumene(29.13 min)

FID

MS

Cumene(29.15 min)

Qualitative analysis based on the mass spectrum displayed

6

Page 8: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

ApplicationNews

No.M268

Gas Chromatography Mass Spectrometry

Analysis of Residual Solvents – Class 1, Class 2A, Class 2B – in Pharmaceuticals Using Headspace-GC/MS

LAAN-A-MS-E034

Residual solvents in pharmaceuticals are defined as organic volatile chemicals that are used or produced in the manufacture of drug substances or excipients, or in the preparation of drug products. Residual solvents are classified and managed as Class 1 to Class 3 substances, depending on the risk they pose to human health.According to the USP, "General Chapter <467> Residual Solvents" method, analysis of these residual solvents is to be conducted by the headspace GC-FID method (HS-GC). However in this application, we investigated using headspace-GC/MS (HS-GC/MS) according to Procedure A. Using the HS-GC method, measurement is to be performed as three separate analyses, which are required to achieve chromatographic separation within the three different classes of compounds, Class 1, Class 2A, and Class 2B. However, using HS-GC/MS, complete chromatographic separation is not necessary, so all the compounds can be analyzed in a single run. In addition, compound confirmation and qualitative information of unknown peaks can also be obtained.

n Sample PreparationThe Class 1, Class 2A, and Class 2B aqueous standard solutions were prepared so that the concentrations become the same as standard solution designated in the "USP <467> Residual Solvents" method.

Headspace Sampler : HS-20

Gas Chromatograph Mass Spectrometer : GCMS-QP2010 UltraHSMode : Loop (Volume: 1 mL)Oven Temperature : 80 °CSample Line Temperature : 150 °CTransfer Line Temperature : 150 °CGas Pressure for Vial Pressurization : 100 kPaVial Equilibrating Time :60 minVial Pressurizing Time :2.0 minPressure Equilibrating Time :0.1 minLoad Time :0.1 minLoad Equilibrating Time :0.1 minInjection Time :0.5 minNeedle Flush Time :5.0 minGC

Column : Rxi-624sil MS (30 m × 0.25 I.D.,1.4 µm)

Injection Mode :Split Split Ratio :1:30Control Mode :Constant linear velocity (35 cm/sec)Oven Temperature :40 °C (20 min) → 10 °C/min →

240 °C (20 min)

MSIon Source Temperature : 200 °CInterface Temperature : 250 °CSCAN Range :m/z 29 ~ 200SIM Conditions : Table 1Event Time : SIM 0.2 sec, SCAN 0.3 sec

Compound Name Target Ident 1 Ident 2

Class 1 1,1-Dichloroethene 61 96

1,1,1-Trichloroethane 97 99

Carbon Tetrachloride 117 119

Benzene 78 77 51

1,2-Dichloroethane 62 64

Class 2A Methanol 31 29

Acetonitrile 40 39

Methylene chloride 84 86

trans-1,2-Dichloroethene 96 61

cis-1,2-Dichloroethene 96 61

Tetrahydrofuran 72 42

Cyclohexane 84 56

Methylcyclohexane 98 83

1,4-Dioxane 88 58

Toluene 91 92

Chlorobenzene 112 77

Ethylbenzene 91 106

m,p-Xylene 91 106

o-Xylene 91 106

Class 2B n-Hexane 86 56

Nitromethane 30 46

Chloroform 83 85

1,2-Dimethoxyethane 45 29

Trichloroethene 130 132

Pyridine 79 52

2-Hexanone 58 100

Tetralin 104 132n Analytical Conditions

Table 1 SIM Monitoring Ions

n ResultsFig. 1 shows Total Ion Chromatogram (TIC) for the USP Class 1 compounds. Fig. 2 and 3 are the TICs for Class 2A and 2B compounds, respectively. Peaks that cannot be identified in the TIC and peaks that completely or partially co-elute are shown in the extracted ion chromatogram (EIC). Due to the selectivity of the GC/MS, good separation was obtained by using the SIM acquisition mode. Fig. 4, 5 and 6 show the EIC/SIM chromatograms of the individual components. Good peak shapes we re ob ta ined fo r mos t o f the compounds. In addition, an improved signal-to-noise ratio (S/N) was obtained for CCl4 using the HS-GC/MS method, compared to that obtained by the HS-GC method. Repeatability using the HS-GC/MS SIM mode yielded an RSD of 1.3 to 3.9 % (Tables 2, 3, and 4).

n ConclusionUsing the HS-GC/MS method, simultaneous analysis of USP <467> Class 1, Class 2A, and Class 2B compounds was demonstrated without compromising separation, repeatability, or analysis accuracy.Note: Measurement of residual solvents in pharmaceuticals using HS-

GC/MS has not been adopted as an official method.

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ApplicationNews

No.M268

Fig. 2 TIC Chromatogram of Class 2A Solvents

Fig. 3 TIC Chromatogram of Class 2B Solvents

Car

bon

tetra

chlo

ride

tran

s

cis

m,p

o

n

Fig. 1 TIC Chromatogram of Class 1 Solvents

8

Page 10: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

ApplicationNews

No.M268

1,1-Dichloroethene 1,1,1-Trichloroethane Carbon tetrachloride Benzene 1,2-Dichloroethane

EIC

SIM

3.5 4.0

2.5

5.0

(×1,000)

61.0096.00

8.5 9.0

2.5

5.0

7.5(×1,000)

99.0097.00

9.0 9.5

1.0

2.0

(×1,000)

119.00117.00

10.0 10.5

2.5

5.0

(×1,000)

51.0077.0078.00

10.0 10.5

0.5

1.0

1.5(×1,000)

64.0062.00

3.5 4.0

2.5

5.0

7.5

(×1,000)

61.0096.00

8.5 9.0

2.5

5.0

7.5

(×1,000)

99.0097.00

9.0 9.5

1.0

2.0

3.0(×1,000)

119.00117.00

10.0 10.5

2.5

5.0

(×1,000)

51.0077.0078.00

10.0 10.5

0.5

1.0

1.5

(×1,000)

64.0062.00

4.0 4.5

2.5

0.0

(×100,000)

86.0084.00

4.5 5.0

0.5

1.0

(×1,000,000)

61.0096.00

7.0 7.5

2.5

5.0

7.5

(×100,000)

61.0096.00

8.5 9.0

1.0

2.0

(×1,000,000)

56.0084.00

14.5 15.0

2.5

5.0

7.5

(×100,000)

83.0098.00

15.5 16.0

1.0

2.0

(×1,000)

58.0088.00

22.0 22.5

1.0

2.0

(×1,000,000)

92.0091.00

27.0 27.5

1.0

2.0

(×1,000,000)

106.0091.00

27.5 28.0

1.0

2.0

(×1,000,000)

106.0091.00

4.0 4.5

2.5

0.0

(×10,000)

39.0040.0041.00

2.0 2.5

1.0

2.0

3.0(×10,000)

29.0031.00

7.5 8.0

0.5

1.0

(×100,000)

42.0072.00

EIC

EIC

SIM

SIM

Methanol

Toluene

Acetonitrile Dichloromethane trans -1,2-dichloroethene cis -1,2-dichloroethene

Tetrahydrofuran Cyclohexane

EIC

m,p-XyleneChlorobenzene Ethylbenzene o-Xylene

SIM

2.0 2.5

1.0

2.0

3.0(×10,000)

29.0031.00

4.0 4.5

0.5

1.0

(×10,000)

39.0040.00

4.0 4.5

2.5

0.0

(×100,000)

86.0084.00

4.5 5.0

0.5

1.0(×1,000,000)

61.0096.00

7.0 7.5

2.5

5.0

(×100,000)

61.0096.00

7.5 8.0

0.5

1.0(×100,000)

42.0072.00

8.5 9.0

1.0

2.0

(×1,000,000)

56.0084.00

14.5 15.0

2.5

5.0

7.5(×100,000)

83.0098.00

15.5 16.0

1.0

2.0

(×1,000)

58.0088.00

22.0 22.5

1.0

2.0

(×1,000,000)

92.0091.00

26.5 27.0

0.5

1.0

(×1,000,000)

77.00112.00

27.0 27.5

1.0

2.0(×1,000,000)

106.0091.00

27.5 28.0

1.0

2.0(×1,000,000)

106.0091.00

28.0 28.5

2.5

0.0

(×1,000,000)

106.0091.00

26.5 27.0

0.5

1.0

(×1,000,000)

77.00112.00

28.0 28.5

2.5

0.0

(×1,000,000)

106.0091.00

1,4-DioxaneMethylcyclohexane

Fig. 4 EIC/SIM Chromatograms of Class 1 Solvents

Fig. 5 EIC/SIM Chromatograms of Class 2A Solvents

9

Page 11: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

ApplicationNews

No.

For Research Use Only. Not for use in diagnostic procedures.The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu. The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject to change without notice.

© Shimadzu Corporation, 2014www.shimadzu.com/an/

M268

First Edition: Oct. 2014

EIC

SIM

n-Hexane

Tetralin2-Hexanone

Nitromethane

Pyridine

5.0 5.5

2.5

5.0

7.5(×10,000)

56.0086.00

7.0 7.5

2.5

5.0

7.5

(×100)

46.0030.00

8.0 8.5

2.5

5.0

(×10,000)

85.0083.00

10.0 10.5

2.5

5.0

(×1,000)

29.0045.00

13.0 13.5

2.5

0.0

(×10,000)

132.00130.00

21.5 22.0

1.0

2.0

3.0(×1,000)

52.0079.00

25.0 25.5

0.5

1.0

1.5(×10,000)

100.0058.00

5.0 5.5

2.5

5.0

7.5

(×10,000)

56.0086.00

7.0 7.5

2.5

5.0

7.5

(×100)

46.0030.00

8.0 8.5

2.5

5.0

(×10,000)

85.0083.00

10.0 10.5

2.5

5.0

7.5(×1,000)

29.0045.00

13.0 13.5

2.5

5.0(×10,000)

132.00130.00

34.5 35.0

2.5

0.0

(×100,000)

132.00104.00

21.5 22.0

1.0

2.0

3.0

(×1,000)

52.0079.00

25.0 25.5

1.0

0.0

(×10,000)

100.0058.00

34.5 35.0

2.5

0.0

(×100,000)

132.00104.00

EIC

SIM

Trichloroethene1,2-DimetoxyethaneChloroform

Fig. 6 EIC/SIM Chromatograms of Class 2B Solvents

Conc. Area RSD (%)

Compound Name (µg/mL) EIC SIM

Class 1 1,1-Dichloroethene 0.018 2.42 2.79

1,1,1-Trichloroethane 0.033 1.86 2.61

Carbon tetrachloride 0.045 1.64 1.62

Benzene 0.064 1.52 2.01

1,2-Dichloroethane 0.085 2.21 2.30

Conc. Area RSD (%)

Compound Name (µg/mL) EIC SIM

Class 2B n-Hexane 0.52 3.46 3.38

Nitromethane 0.82 3.72 2.44

Chloroform 1.97 2.48 2.67

1,2-Dimethoxyethane 0.42 2.62 2.74

Trichloroethene 0.42 1.23 1.56

Pyridine 1.67 2.94 3.29

2-Hexanone 0.83 0.83 1.34

Tetralin 0.65 1.87 1.77

Conc. Area RSD (%)

Compound Name (µg/mL) EIC SIM

Class 2A Methanol 3.03 4.26 3.83

Acetonitrile 2.85 2.74 3.29

Methylene Chloride 27.0 2.24 2.78

trans-1,2-Dichloroethene 14.6 1.91 2.60

cis-1,2-Dichloroethene 5.05 1.93 2.49

Tetrahydrofuran 3.12 1.87 2.12

Cyclohexane 24.1 1.67 2.27

Methylcyclohexane 8.72 1.33 1.69

1,4-Dioxane 6.15 3.13 2.54

Toluene 7.00 1.17 1.56

Chlorobenzene 2.92 1.30 1.28

Ethylbenzene 1.47 1.32 1.41

m,p-Xylene 2.48 1.07 1.41

o-Xylene 10.3 1.23 1.66

Table 2 Repeatability of Peak Area of Class 1 Solvents (n = 6)

Table 4 Repeatability of Peak Area of Class 2B Solvents (n = 6)

Table 3 Repeatability of Peak Area of Class 2A Solvents (n = 6)

10

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FID

APC PressureControl

Splitting Unit

ApplicationNews

No.M272

Gas Chromatography Mass Spectrometry

Analysis of Residual Solvents in Pharmaceuticals Using Headspace GC-FID/MS Detector Splitting System

LAAN-A-MS-E038

Table 1 Analytical Conditions

Headspace Sampler : HS-20

GCMS : GCMS-QP2020Hydrogen Flame Ionization Detector Splitting System

: FID-2010Plus

HSMode : Loop (volume 1 mL)Oven Temp. : 80 °CSample Line Temp. : 90 °CTransfer Line Temp. : 105 °CGas Pressure for Vial Pressurization : 76.4 kPaVial Equilibrating Time : 45 minVial Pressurizing Time : 2.0 minPressure Equilibrating Time : 0.1 minLoad Time : 0.5 minLoad Equilibrating Time : 0.1 minInjection Time : 0.5 min

Needle Flushing Time : 15.0 minAPC Pressure : 20 kPa

GC

Column : SH Rxi-624sil MS(30 m × 0.32 mm I.D., 1.8 µm)

Injection Mode : Split (split ratio 1:5)Control Mode : Constant Pressure (89.4 kPa) Carrier Gas : HeOven Temp. : 40 °C (20 min) → 10 °C/min →

240 °C (20 min)Restrictor (FID) : 1.1 m × 0.25 mmRestrictor (MS) : 1.5 m × 0.20 mmAPC Pressure : 20 kPa

FID

Temp. : 250 °CMake-Up Flowrate : 30 mL/min (He)Hydrogen Flowrate : 40 mL/minAir Flowrate : 400 mL/min

MS

Ion Source Temp. : 200 °CInterface Temp. : 250 °CSCAN Range : m/z 29 to 250Event Time : 0.3 sec

Headspace gas chromatography with flame ionization detection (GC-FID) is often used for residual solvent testing of pharmaceuticals, though the qualitative power of this method is not particularly high. Because gas chromatography mass spectrometry (GC/MS) utilizes MS to perform qualitative analysis based on mass spectra, GC/MS can be used to estimate and identify individual peaks detected in the expected vicinity of a target solvent as well as other unknown peaks.We describe an example of residual solvent test of a pharmaceutical using a detector splitting system that simultaneously obtains FID and MS data in a single measurement.

n Sample PreparationAccording to Water-Soluble Articles, Procedure A, in USP <467>, we prepared a class 1 standard solution, class 2 standard solution A, class 2 standard solution B, test solution, and class 1 system suitability solution. An active pharmaceutical ingredient was used for the test solution sample.

n Analytical ConditionsThe image of the Shimadzu GCMS-QP2020/FID detector splitting system is shown in Fig. 1, and analytical conditions are shown in Table 1. Headspace conditions were determined based on USP <467>. The column outlet was split between FID and MS, and MS was performed in scanning mode. Using Shimadzu's Advanced Flow Technology Software to determine the splitting ratio, the flowrate ratio was optimized to FID:MS of 1:1.

Fig. 1 System Image11

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ApplicationNews

No.M272

n ResultsFig. 2 to 5 show the FID and MS chromatograms obtained for class 1 standard solution, class 2 standard solution A, class 2 standard solution B, and class 1 system suitability solution.

3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0

0

1000

2000

3000

4000

5000

6000

1, 1

-Dic

hlor

oeth

ene

1, 1

, 1-T

richl

oroe

than

e

Car

bon

Tetr

achl

orid

e

Benz

ene

1, 2

-Dic

hlor

oeth

ane

MS (Scan) FID

2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5

25000

50000

75000

100000

125000

150000

175000

200000

225000

Met

hano

l

Ace

toni

trile

Met

hyle

neC

hlor

ide

tran

s-1,

2-D

ichl

oroe

then

e

cis-

1, 2

-Dic

hlor

oeth

ene

Tetr

ahyd

rofu

ran

Cyc

lohe

xane

Met

hylc

yclo

hexa

ne

1, 4

-Dio

xane

Tolu

ene

Chl

orob

enze

neEt

hylb

enze

ne

m,p

-Xyl

ene

o-X

ylen

eC

umen

e

5.0 10.0 15.0 20.0 25.0 30.0 35.0

2500

7500

10000

12500

15000

17500

20000

N-H

exan

e

Nitr

omet

hane

Chl

orof

orm

1, 2

-Dim

etho

xyet

hane Tr

ichl

oroe

then

e

Pyrid

ine 2-

Hex

anon

e

Tetr

alin

Fig. 2 Chromatograms of Class 1 Standard Solution

Fig. 3 Chromatograms of Class 2 Mixture A Standard Solution

Fig. 4 Chromatograms of Class 2 Mixture B Standard Solution

12

Page 14: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

ApplicationNews

No.M272

MS(Scan) FID

3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0

1, 1

-Dic

hlor

oeth

ene

1, 1

, 1-T

richl

oroe

than

e

Car

bon

Tetr

achl

orid

e

Benz

ene

1, 2

-Dic

hlor

oeth

ane

Fig. 5 Chromatograms of Class 1 System Suitability Solution

To check the mass spectra of the peaks detected by FID, the peak retention times in chromatograms obtained by FID and MS must match as closely as possible. Looking at Fig. 2 to 4 show all the peak retention times are lined up, from the earliest to the latest constituent.When using a detector splitting system, the two detectors must detect the same peaks detected by normal gas chromatography. In other words, detector splitting systems are expected to have the equivalent system performance as a normal analytical system. Procedure A in USP <467> states the two items below concerning system suitability. We attempted to confirm the two items below for the detector splitting system, and for the repeatability of class 1 standard solution analysis.

(1) Detector confirmationThe S/N ratio of 1, 1, 1-trichloroethane in class 1 standard solution is 5 or higher; the S/N ratio of each peak in class 1 system suitability solution is 3 or higher.

(2) System performanceThe peak resolut ion between acetonit r i le and dichloromethane in class 2 standard solution is 1.0 or higher.

The results (FID S/N ratios) of analyzing class 1 standard solution and class 1 system suitability solution with the detector splitting system are shown in Table 2, and the repeatability results (FID repeatability) of analyzing class 1 standard solution are shown in Table 3. These results show the detector sp l i t t ing system meets the performance required of a standard system. The peak resolution of acetonitrile and dichloromethane in class 2 standard solution was 2.37, showing this system is also suitable in terms of resolution.

Table 2 Signal-to-Noise Ratio in Class 1 Standard Solution and System Suitability Solution

Table 3 Repeatability in Class 1 Standard Solution (n=6)

Compound Standard solutionSolution for system

suitability test1, 1-Dichloroethene 221.9 141.41, 1, 1-Trichloroethane 117.6 82.2Carbon tetrachloride 10.2 7.6Benzene 106.3 56.81, 2-Dichloroethane 26.4 14.2

Compound Relative standard deviation (%)1, 1-Dichloroethene 1.61, 1, 1-Trichloroethane 2.2Carbon tetrachloride 1.8Benzene 3.51, 2-Dichloroethane 2.9

13

Page 15: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

5.0 10.0 15.0 20.0 25.0 30.0 35.0

5.0 10.0 15.0 20.0 25.0 30.0 35.0

5.0 10.0 15.0 20.0 25.0 30.0 35.0

5.0 10.0 15.0 20.0 25.0 30.0 35.0

ab

d

c

Class1 Standard(FID)

Class2A Standard(FID)

Class2B Standard(FID)

Test (FID)

Test (MS)

50 100 150 200 2500

50

10056.031.0 n-Butanol

50 100 150 200 2500

50

10043.0

29.0

61.088.1

Ethyl acetate

50 100 150 200 2500

50

10091.1

106.2

77.051.0

o-Xylene

50 100 150 200 2500

50

10057.0

41.0 87.173.1 130.2

Dibutylether

ApplicationNews

No.

© Shimadzu Corporation, 2016

For Research Use Only. Not for use in diagnostic procedure. This publication may contain references to products that are not available in your country. Please contact us to check the availability of these products in your country. The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu. Company names, product/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation or its affiliates, whether or not they are used with trademark symbol “TM” or “®”. Third-party trademarks and trade names may be used in this publication to refer to either the entities or their products/services. Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own.

The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject to change without notice.

www.shimadzu.com/an/

M272

First Edition: Jul. 2016

The results (chromatograms) of analyzing active pharmaceutical ingredients in the detector splitting system are shown in Fig. 6, and the mass spectra of detected peaks are shown in Fig. 7 to 9. Peaks a and b, based on their respective mass spectra (Fig. 7 and 8), were estimated to be ethyl acetate and butanol. Both these constituents are low toxicity class 3 solvents.

Though its peak strength is smaller than that observed in the standard solution, a peak was also detected at the elution position of o-xylene (c). Checking the mass spectrum of this peak (Fig. 9) showed it differed from the mass spectrum of xylene (peak d, Fig. 10), and was estimated to be dibutyl ether.

Fig. 6 Chromatograms of Standard Solutions and Test Solutions

Fig. 7 Mass Spectrum of Peak a Fig. 9 Mass Spectrum of Peak c

Fig. 8 Mass Spectrum of Peak b Fig. 10 Mass Spectrum of Peak d

n ConclusionAn FID and MS detector splitting system obtains FID and MS data simultaneously in a single analysis, and can be used as a simpler method of confirming constituent identity. This system shows promise for use in residual solvent testing of pharmaceuticals.Note: Reference USP <467>This data was obtained by a method that does not conform to the pharmacopoeia, as analytical conditions based on USP <467> was modified before use.

14

Page 16: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

C146-E300

Gas Chromatograph Mass Spectrometer

Ultra High Speed GC-MS That Offersa Dramatic Leap in Sensit iv i ty and Product iv i ty

Provides Higher Sensitivity and Reduced Operation Costs

The high-sensitivity, high-speed capability analysis is achieved, using helium, hydrogen or nitrogen as the

carrier gas and the ionization is easily switched without stopping the MS.

Dramatic Improvement in the Ef�ciency of Multicomponent Simultaneous Analysis

The GCMS Insight software package supports everything from method creation to analysis.

Databases with Retention Indices to Support Analysis

Databases are available to satisfy a variety of needs, including environmental analysis and food analysis, etc.

Con�gure Optimal Analysis Systems to Meet Your Needs

It is possible to con�gure a system to suit your application, including the form of the samples, and the

features and concentrations of the components.

15

Page 17: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

Provides High-Sensitivity and FunctionalityUnder a Variety of Analytical Conditions

The GCMS-QP2020 adopts a new differential exhaust turbomolecular

pump with heightened exhaust efficiency; as a result, in addition to

helium, the system can now be operated with hydrogen or nitrogen

as the carrier gas. In addition, the system supports a variety of analysis

conditions, including high-speed scan.

(×10,000)

6.00 6.25 6.50 6.75

2.00

1.75

1.50

1.25

1.00

0.75

0.50

0.25

191.00193.00

Chloroneb

Mass chromatograms of pesticides with hydrogen carrier gas (5ppb, SIM)

Even though confirmation of molecular related ions is difficult with

the EI method, data can be acquired by Quick-CI immediately without

stopping the MS.

50 100 150 200 2500

50

100

%86

44 14912165 9141

50 100 150 200 2500

50

100

%236

86218149 18871 91 121

EI Mass Spectrum (Top) and CI Mass Spectrum (Bottom) for Pentylone, a Typeof Cathinone

Numerous Databases Support Analysis

Databases are available to satisfy a variety of needs, including

environmental analysis, foods analysis, off-flavor analysis, and forensic

analysis. All of the databases include retention indices, which support

more accurate qualitative analysis, convenient quantitative method

development, and screening analysis.

Retention Indices

SimultaneousAnalysis Database

Smart MetabolitesDatabase

Off-FlavorDatabase

Pesticide Library

FFNSC Flavor andFragrance Library

Forensic ToxicologyDatabase

Achieves High-Sensitivity and Efficiency ofMulticomponent Analysis

The GCMS Insight software package supports everything from method

creation to analysis. The Smart SIM functionality automatically creates

SIM programs that enable measurements of multiple components

with high sensitivity. In addition, a special data analysis program,

increases data processing efficiency.

Smart SIM

The optimal MS table isautomatically created

SIM method file

Data analysis program LabSolutions Insight

Configure a Range of Diverse Systems

It is possible to configure a system to suit your application, including

the form of the samples being analyzed, and the features and

concentrations of the components being measured. All the

peripherals comprising the system units are supported by Shimadzu,

so you can secure about using them.

HS-20

OPTIC-4EGA/PY-3030D AOC-6000 TD-20*

GC×GC

MDGC

* Not available in the U.S.

www.shimadzu.com/an/

Company names, product/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation or its af�liates, whether or not they are used with trademark symbol “TM” or “®”.Third-party trademarks and trade names may be used in this publication to refer to either the entities or their products/services. Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own.

For Research Use Only. Not for use in diagnostic procedures. The contents of this publication are provided to you “as is” without warranty of any kind, and are subject to change without notice. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication.

© Shimadzu Corporation, 2015

Printed in Japan 3655-11508-30ANS16

Page 18: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

High ReproducibilityThe HS-20 Series achieves high reproducibility through both high-accuracy flow rate

control via the pneumatic flow controller (Advanced Flow Control: AFC™ system) and

a mechanism that allows sample vial to enter the oven from the bottom.

Consequently, this system minimizes heat loss, and maintains high thermal stability

during overlap analyses.

Low CarryoverKeeping the sample line inert and as short as possible results in extremely low

carryover. No residue is left, even with acetic acid and other polar compounds,

enabling highly reliable analysis. (Patent pending)

High-Temperature CompatibilityWith an oven configurable up to 300 °C and a simple, inert

sample line, the HS-20 Series allows the analysis of

high-boiling compounds.

Cyclic siloxane is a raw silicone material, trace quantities of

which remain in oils, liquid rubber, and other products.

Because cyclic siloxane is volatile, it could potentially cause

problems with contacts in electronic parts, so controlling its

concentration is very important. The HS-20 Series makes it

possible to measure everything from cyclic siloxane to

phthalate esters under the same conditions.

Typical HS SamplerInternal heat easily escapes during vial transfer, temporarily reducing the oven temperature.

HS-20Conveyance from the bottom makes it difficult for heat to escape from inside, improving oven temperature stability. (Patent pending)

Cyclic siloxane C2nH6nOnSin (m/z 73) in resin outgas at 300 °C

Loop fillingvent line

Methanol 50 ppmreproducibility (n = 20)1.5 %

n-Butanol 50 ppmreproducibility (n = 20)1.5 %

Vial pressurizing line

Residual acetic acid in coffee< 0.0001 %

Residual DMI solvent< 0.0001 %

CoffeeBlank

DMI solventBlank

Acetic acid DMI

Sample warmed to a constant temperature of 300°C

Sample warmed to a constant temperature of 220°C

n=5 6 7 8 9 10 11 12 13 14 15 16

The HS-20 Series is the optimal solution for volatile component analysis.

Its superior performance and user-friendly design support all types of analyses, from research

to quality control.

HS-20 Series of Headspace SamplersA Revolutionary System Aimed at Performance and Ease of Use

With the trap model, concentrating the headspace gas

enables the analysis of ultra-trace components, such as

gases released from parts and materials.

The optional barcode reader enables samples to be

controlled via a chromatography data system.

Excellent Expandability

Easily place samples in the tray with the user-friendly

design. Also, the needle, sample loop, trap, and other

consumables can easily be replaced from the top of the

instrument.

User-Friendly Design

High reproducibility and low carryover ensure reliable

quantitation. In addition, an oven with a maximum

temperature of 300 °C enables analysis of high-boiling

compounds.

Excellent Performance

3

2

1

• Electronic cooling trap (trap model)• Barcode reader option

• User-friendly sample tray• Easy maintenance

• High reproducibility • Low carryover• High-temperature compatibility

Excellent Performance

7.0 8.0 9.0 10.0 11.0 12.0 min 28.0 28.25 28.5 28.7529.0029.2529.50min

HS-20 SeriesHeadspace Samplers2 318

Page 19: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

High ReproducibilityThe HS-20 Series achieves high reproducibility through both high-accuracy flow rate

control via the pneumatic flow controller (Advanced Flow Control: AFC™ system) and

a mechanism that allows sample vial to enter the oven from the bottom.

Consequently, this system minimizes heat loss, and maintains high thermal stability

during overlap analyses.

Low CarryoverKeeping the sample line inert and as short as possible results in extremely low

carryover. No residue is left, even with acetic acid and other polar compounds,

enabling highly reliable analysis. (Patent pending)

High-Temperature CompatibilityWith an oven configurable up to 300 °C and a simple, inert

sample line, the HS-20 Series allows the analysis of

high-boiling compounds.

Cyclic siloxane is a raw silicone material, trace quantities of

which remain in oils, liquid rubber, and other products.

Because cyclic siloxane is volatile, it could potentially cause

problems with contacts in electronic parts, so controlling its

concentration is very important. The HS-20 Series makes it

possible to measure everything from cyclic siloxane to

phthalate esters under the same conditions.

Typical HS SamplerInternal heat easily escapes during vial transfer, temporarily reducing the oven temperature.

HS-20Conveyance from the bottom makes it difficult for heat to escape from inside, improving oven temperature stability. (Patent pending)

Cyclic siloxane C2nH6nOnSin (m/z 73) in resin outgas at 300 °C

Loop fillingvent line

Methanol 50 ppmreproducibility (n = 20)1.5 %

n-Butanol 50 ppmreproducibility (n = 20)1.5 %

Vial pressurizing line

Residual acetic acid in coffee< 0.0001 %

Residual DMI solvent< 0.0001 %

CoffeeBlank

DMI solventBlank

Acetic acid DMI

Sample warmed to a constant temperature of 300°C

Sample warmed to a constant temperature of 220°C

n=5 6 7 8 9 10 11 12 13 14 15 16

The HS-20 Series is the optimal solution for volatile component analysis.

Its superior performance and user-friendly design support all types of analyses, from research

to quality control.

HS-20 Series of Headspace SamplersA Revolutionary System Aimed at Performance and Ease of Use

With the trap model, concentrating the headspace gas

enables the analysis of ultra-trace components, such as

gases released from parts and materials.

The optional barcode reader enables samples to be

controlled via a chromatography data system.

Excellent Expandability

Easily place samples in the tray with the user-friendly

design. Also, the needle, sample loop, trap, and other

consumables can easily be replaced from the top of the

instrument.

User-Friendly Design

High reproducibility and low carryover ensure reliable

quantitation. In addition, an oven with a maximum

temperature of 300 °C enables analysis of high-boiling

compounds.

Excellent Performance

3

2

1

• Electronic cooling trap (trap model)• Barcode reader option

• User-friendly sample tray• Easy maintenance

• High reproducibility • Low carryover• High-temperature compatibility

Excellent Performance

7.0 8.0 9.0 10.0 11.0 12.0 min 28.0 28.25 28.5 28.7529.0029.2529.50min

HS-20 SeriesHeadspace Samplers2 319

Page 20: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

Sample ConcentrationThe HS-20 trap model is equipped with an electronic cooling trap that concentrates the headspace gas, enabling

high-sensitivity analysis. By using hydrophobic Tenax, the trap enables the analysis of low-boiling compounds by

concentrating them to high-boiling compounds in samples containing moisture.

Method files make it easy to switch between trap and conventional modes, in which a sample loop is used. The two modes

can be combined even in continuous analysis via batch processing.

High-Sensitivity Analysis of Fragrance Components in CoffeeIn combination with a GCMS, the high-sensitivity electronic cooling trap enables qualitative and quantitative analyses of

fragrance components at trace levels undetectable with a conventional headspace sampler.

User-Friendly Sample TrayThe HS-20 sample tray is 20 cm higher than the desk,

enabling it to be seen at all times. This makes sample

placement easy.

In addition, 10 mL and 20 mL vials can be placed and

analyzed simultaneously without the need for special

attachments.

Furthermore, the optional barcode reader allows samples to

be controlled using barcodes.

Easy MaintenanceThe HS-20 Series has been designed to enable sample loop and needle

replacement and other maintenance work to be performed easily from the top of

the instrument.

Even if sample lines become contaminated by high-concentration samples, the

piping alone can now be replaced.

Also, the capillary column joints are shared with the GC sample injection unit,

enabling easy column replacement.

This superior design minimizes downtime during maintenance and improves

laboratory productivity.

Analysis of blood and other samples in the forensic field requires a system that not only offers excellent performance, but

also eliminates operational errors.

With its user-friendly design, the HS-20 Series prevents mistakes, while the barcode reader records logs to dramatically

improve traceability.

The instrument can be controlled by the CFR 21 Part 11-compliant LabSolutions chromatography data system, ensuring

traceability of analysis conditions and operations. In addition, an automatic shutdown function operates after analysis is

completed, saving electricity and carrier gas. (LabSolutions LC/GC only. Not supported by GCMS software.)

Area(x100,000)

5.5

5.0

4.5

4.0

3.5

3.0

2.5

2.0

1.5

1.0

(x1,000,000)

1.1

0 10 20 30 40 50 60 70 80 90 Concentration

1.0

0.9

0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0.0

Methylfuran

Aceticacid

Acetol

Pyridine

Methylpyrazine

Furfurylalchol

2,5 -Dimethylpirazine

Furfurylacetate

Peak areas are improved 5 to 50 times.

6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0

Electronic Cooling Trap Unit Switching Between Loop Mode and Trap Mode Using Batch Editor

1ppt TCA in Wine (Loop mode)

User-Friendly Design Excellent Expandability

Quantitative Results Browser

Area × 4S/N × 10

2,4,6-TCA 2,4,6-TCA

1ppt TCA in Wine (Trap mode) Calibration Curve from TCA Added to Wine (trap mode)

1~100pptR 0.998

HS-20Trap + GCMS-QP2010 Ultra

4 5HS-20 Series

Headspace Samplers20

Page 21: Shimadzu · capabilities will elevate your lab to the next level. Designed with the Analyst in Mind An advanced interface enables intuitive operation with clear graphics. Shimadzu's

Sample ConcentrationThe HS-20 trap model is equipped with an electronic cooling trap that concentrates the headspace gas, enabling

high-sensitivity analysis. By using hydrophobic Tenax, the trap enables the analysis of low-boiling compounds by

concentrating them to high-boiling compounds in samples containing moisture.

Method files make it easy to switch between trap and conventional modes, in which a sample loop is used. The two modes

can be combined even in continuous analysis via batch processing.

High-Sensitivity Analysis of Fragrance Components in CoffeeIn combination with a GCMS, the high-sensitivity electronic cooling trap enables qualitative and quantitative analyses of

fragrance components at trace levels undetectable with a conventional headspace sampler.

User-Friendly Sample TrayThe HS-20 sample tray is 20 cm higher than the desk,

enabling it to be seen at all times. This makes sample

placement easy.

In addition, 10 mL and 20 mL vials can be placed and

analyzed simultaneously without the need for special

attachments.

Furthermore, the optional barcode reader allows samples to

be controlled using barcodes.

Easy MaintenanceThe HS-20 Series has been designed to enable sample loop and needle

replacement and other maintenance work to be performed easily from the top of

the instrument.

Even if sample lines become contaminated by high-concentration samples, the

piping alone can now be replaced.

Also, the capillary column joints are shared with the GC sample injection unit,

enabling easy column replacement.

This superior design minimizes downtime during maintenance and improves

laboratory productivity.

Analysis of blood and other samples in the forensic field requires a system that not only offers excellent performance, but

also eliminates operational errors.

With its user-friendly design, the HS-20 Series prevents mistakes, while the barcode reader records logs to dramatically

improve traceability.

The instrument can be controlled by the CFR 21 Part 11-compliant LabSolutions chromatography data system, ensuring

traceability of analysis conditions and operations. In addition, an automatic shutdown function operates after analysis is

completed, saving electricity and carrier gas. (LabSolutions LC/GC only. Not supported by GCMS software.)

Area(x100,000)

5.5

5.0

4.5

4.0

3.5

3.0

2.5

2.0

1.5

1.0

(x1,000,000)

1.1

0 10 20 30 40 50 60 70 80 90 Concentration

1.0

0.9

0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0.0

Methylfuran

Aceticacid

Acetol

Pyridine

Methylpyrazine

Furfurylalchol

2,5 -Dimethylpirazine

Furfurylacetate

Peak areas are improved 5 to 50 times.

6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0

Electronic Cooling Trap Unit Switching Between Loop Mode and Trap Mode Using Batch Editor

1ppt TCA in Wine (Loop mode)

User-Friendly Design Excellent Expandability

Quantitative Results Browser

Area × 4S/N × 10

2,4,6-TCA 2,4,6-TCA

1ppt TCA in Wine (Trap mode) Calibration Curve from TCA Added to Wine (trap mode)

1~100pptR 0.998

HS-20Trap + GCMS-QP2010 Ultra

4 5HS-20 Series

Headspace Samplers21

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Batch Analysis of VOCs in WastewaterWith its high thermal stability and inert sample line, the HS-20 Series can measure VOCs in wastewater with high

reproducibility. Carryover is minimal, so the sample tray, which is capable of holding 90 samples, can be effectively

utilized.

Aqueous Solution of USP467 Class 2A/2B Pharmaceutical Residual SolventsIn combination with a robust GC detector, the system can be used for quality control requiring high quantitative

accuracy. Traceability is guaranteed by the all-sample leak check function and the digitized log function.

4.0

min

5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0

1

2

3 4 5

6 7 8

9

10 11

12 13

14

15

17 16

18

19

20

21

22

2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5 30.0 32.5 35.0

min2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5 30.0 32.5 35.0

Sample Injection Method

Number of Vials

Vials

Vial Mixing

Leak Check

Optional Barcode Reader

Vial Warming Temperature

Sample Line Temperature

Transfer Line Temperature

Trap

Trap Cooling Temperature

Trap Heating Temperature

Carrier Gas Control

Vial Pressurized-Gas Control

Carrier Gas and Vial Pressurizing Gas

PC Interface

Control Software

Software Operating Environment

Guaranteed Operating Environment

Power Supply

Dimensions

Weight

Sulfinert sample loop 1 mL (standard); 0.2 mL, 3 mL (optional) or trap (HS-20Trap)

90

Outer dia. 22.5 mm × 79 mm (20 mL); outer dia. 22.5 mm × 46 mm (10 mL); can be combined

5 stages max.

All-vial automatic check

Optional, can read 6 types of barcodes

Room temperature + 10 to 300 °C (Settings are 0 to 300 °C, in 1 °C units, with an accuracy of ±0.1 °C)

Room temperature + 10 to 220 °C or 150 to 300 °C (set in 1 °C units, accuracy of ±0.5 °C)

Long transfer line model (HS-20LT): Room temperature + 10 to 220 °C

Room temperature + 10 to 350 °C (set in 1 °C units, accuracy of ±0.5 °C)

Long transfer line model (HS-20LT): Room temperature + 10 to 200 °C

Inner dia. 2 mm × 100 mm, Sulfinert tube

Filler TenaxTA (standard), Carbopack + Carboxene (optional)

-30 to 80 °C (set in 1 °C units, accuracy of ±1 °C)

For a sample line at 250 to 300 °C, room temperature - 30 °C

For 150 to 250 °C, room temperature - 40 °C

For 150 °C or less, room temperature - 50 °C

0 to 350 °C (set in 1 °C units, accuracy of ±1 °C)

Electronic control via AFC built into GC

Electronic control via APC built into GC

High-purity helium or nitrogen

USB

Operates collectively with LabSolutions LC/GC (FDA CFR 21 Part 11 compliant)

HSS Control Software is used for GCMS.

Windows XP, Windows Vista, Windows 7 (32/64-bit)

15 to 30 °C, humidity up to 70 % RH (performance guaranteed at 18 to 28 °C with temperature

fluctuations within ±1.3 °C)

1200 VA max. (HS-20, HS-20LT), 1500 VA max. (HS-20Trap)

W553 mm × H430 mm × D543 mm, excluding PC

33 kg (HS-20, HS-20LT), 40 kg (HS-20Trap)

1. 1,1-Dichloroethene 2 Dichloromethane

3 trans-1,2-Dichloroethene

4 cis-1,2-Dichloroethene5 Chloroform

6 1,1,1-Trichloroethane7 Carbon tetrachloride

8 1,2-Dichloroethane9 Benzene

10 Trichloroethene

11 1,2-Dichloropropane

12 Bromochloroethane

13 cis-1,3-Dichloropropane

14 Toluene 15 trans-1,3-Dichloropropane

16 1,1,2-Trichloroethane17 Tetrachloroethene

18 Dibromochloromethane

19 m+p-Xylene20 o-Xylene

21 Bromoform22 1,4-Dichlorobenzene

1.83.0

1.4

2.82.3

1.72.2

2.70.7

1.2

3.1

2.0

1.8

1.41.8

2.90.8

2.1

1.71.4

2.31.2

Reproducibility of USP467 Class 2A/2B Procedure A(Aqueous Solution) RSD% (n=20) 2 Acetnitrile 1.1

3 Dichloromethane 1.7

4 trans-1,2-Dichloroethene 2.3 5 cis-1,2-Dichloroethene 1.9

6 THF 0.6 10 Toluene 2.5

11 Chlorobenzene 2.5

18 1,2-Dimethoxyethane 3.1

20 Pyridine 2.6

Transfer line

HS-20Model

VOC 0.1 ppb reproducibility RSD% (n = 5)

HS-20LTHS-20Trap

Trap NoNo Yes

Long (200 °C)Short (350 °C)Short (350 °C)

HS-20 + GC-2010 Plus

HS-20 HS-20Trap19

17

18

16

15

14

13

12

11

10

20

8 +9

7

6

5 4

3

2

1

IS IS

21

22

6 7HS-20 Series

Headspace Samplers

1418

440

543

Dimensions (HS-20Trap + GCMS-QP2010 Ultra) units: mm

Specifications and Installation Conditions

22