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Application News Nexis GC‐2030 with HS‐20 Next Industry Standard Nexis GC-2030 with HS-20 made drug substance residual solvent analysis simpler with constant flow mode Introduction: Method transfer is no more challenge to Shimadzu new Nexis GC-2030 with HS-20 sampler for residual solvent analysis in drug substance as Nexis GC-2030 can now run in constant flow as an additional carrier gas flow mode. This enables smooth method transfer between different makes of GC. Furthermore, GC-2030 can use the constant linear velocity and constant pressure modes with multistage programing. All control modes can be used with advanced flow technologies, such as backflush, detector switching which leads to better gains in productivity. In this application, data obtained from Make A for the residual solvents analysis of drug substance Sitagleptin was compared with the data generated on Nexis GC-2030 coupled with HS-20 to ascertain repeatability and no carry over during method transfer. Experimental: Multiple residual solvent standard was selected to establish ease of method transfer on Nexis GC-2030 coupled with HS-20. Retention time, area %RSD and carryover test were compared. Sample preparation: Weighed and dissolved 0.3 g methanol, 0.5 g ethanol, 0.5 g isopropyl alcohol, 0.041 g acetonitrile, 0.06 g dichloromethane, 0.5 g tert-butyl methyl ether, 0.5 g ethyl acetate and 0.625 g triethylamine in dimethylacetamide (DMAC) in a 100 mL volumetric flask (DIL-1). Diluent blank preparation : 0.1 g piperazine + 1.0 mL DMAC in 20 mL headspace vial. STD Preparation for RSD check : 0.1 g piperazine + 1.0 mL Std. (DIL-1) in 20 mL headspace vial. The final batch was submitted as: 1. 2 Diluent blank vials 2. 6 Vials for RSD check 3. 2 Diluent blank vials for carry over check Analytical Conditions: No. GC-19-ADI-037 Headspace parameters: Chromatographic parameters: Mode Loop Oven Temp. 75 ⁰C Sample Line Temp. 85 ⁰C Transfer Line Temp. 95 ⁰C Shaking Level 5 Equilibrating Time 20.0 min Pressurize Gas Pressure 103 kPa Load Time 0.5 min Injection Time 1.0 min GC Cycle Time 35.33 min Column SH-Rtx-624 (30 m x 0.32 mm x 1.8 μm) Column Flow 0.5 mL/min Flow Mode: Constant Flow Split Ratio 10.0 Carrier gas Helium Column oven program Rate ⁰C /min Temperature ⁰C Hold Time (min) 40.0 10.0 15.0 180.0 6.0 FID temperature 270 ⁰C APC Pressure programming Rate kPa/min Pressure(kPa) Hold Time (min) 103.0 2.0 50.00 350.0 18.39
Application Data Sheet Application News GC-19-ADI-037 Figure 1: Comparative chromatographic peak profile on Make A of GC-HS and Shimadzu Nexis GC-HS Sr.No. Solvent RT in min. Make A GC-HS RT in min. Shimadzu GC-HS RT Difference in min. 1 Methanol 7.274 7.029 0.245 2 Ethanol 9.696 9.625 0.071 3 Isopropyl Alcohol 11.449 11.488 0.039 4 Acetonitrile 11.859 11.852 0.007 5 Dichloromethane 12.249 12.275 0.026 6 Tert-Butyl Methyl Ether 12.859 12.942 0.083 7 Ethyl Acetate 14.889 14.987 0.098 8 Triethylamine 16.262 16.399 0.137 Table 1: Comparison summary of Retention times (RT) 0.0 2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 min 0 uV RSD Check-6_008.gcd FID RSD Check-6_008.gcd FID Methanol/7.026 Ethanol/9.627 Isopropyl Alcohol/11.495 Acetonitrile/11.856 Dichloromethane/12.277 Tert- Butyl Methyl Ether/12.945 Ethyl Acetate/14.988 Triethylamine/16.397 Make A of GC-HS sampler in constant flow mode Shimadzu GC-2030 with HS-20 sampler in constant flow mode
Application N0. News GC-19-ADI-037 Results and Discussion: The method transfer was very much easy with new advance flow and pressure controller (AFC & APC) that have been developed in Nexis GC-2030 which includes a own CPU. It supports carrier gas constant linear velocity control, constant flowrate control, constant pressure control, and various other control modes which achieves exceptionally high reproducibility for ultra-high-speed and ultra-high-precision control modes. Comparative chromatographic peak profile and summary of retention times are shown in Figure 1 and Table 1 respectively. Figure 2 depicts no carry over for any solvents and Table 2 shows area %RSD and carry over for mixture of residual solvent standard. Sr.No. Solvent Conc. in ppm Area %RSD (n=6) Carryover 1 Methanol 300 2.15 Nil 2 Ethanol 500 2.11 Nil 3 Isopropyl Alcohol 500 2.06 Nil 4 Acetonitrile 41 2.14 Nil 5 Dichloromethane 60 4.32 Nil 6 Tert-Butyl Methyl Ether 500 1.73 Nil 7 Ethyl Acetate 500 1.79 Nil 8 Triethylamine 625 1.65 Nil Table 2 Area %RSD and carryover summary Conclusion: 1. With the new advance flow and pressure controller (AFC & APC) in Nexis GC-2030, it is very easy to adopt any flow control modes to achieve trace level results that are highly reproducible. 2. Very short transfer line in headspace sampler ensures least or no carry over which is the characteristics feature of Shimadzu’s HS-20 headspace system. 3. Constant flow mode made method transfer very easy for residual solvent analysis without any compromise on reproducibility and sensitivity. Copyright © 2013 SHIMADZU ANALYTICAL (INDIA) PVT. LTD. All rights reserved. No part of this document may be reproduced in any form or by any means without permission in writing from SHIMADZU ANALYTICAL (INDIA) PVT. LTD. Shimadzu Analytical (India) Pvt.Ltd. 1 A/B, Rushabh Chambers, Makwana Road, Marol, Andheri (East), Mumbai- 400059, India. Tel: +91 22 29204741 Fax: +91 22 29205679 www.shimadzu.in 0.0 2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 min uV Diluent Blank for Carryover-1_009----.gcd FID RSD Check-6_008.gcd FID Diluent Blank for Carryover-1_009----.gcd FID RSD Check-6_008.gcd FID Methanol/7.026 Ethanol/9.627 Isopropyl Alcohol/11.495 Acetonitrile/11.856 Dichloromethane/12.277 Tert- Butyl Methyl Ether/12.945 Ethyl Acetate/14.988 Triethylamine/16.397 No carryover of Triethylamine Figure 2: Overlay of Standard solvent mixture and diluent blank on Nexis GC-2030 with HS-20 For Research Use Only. Not for use in diagnostic procedures. Contents and/or instrumentations in this application may not available in some countries under each regulation. Please contact the local representatives in details.
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