Determination of Residual Solvents in Thymopentin Drug Substances by Gas Chromatography
Objective The purpose of this study is to adopt headspace gas chromatography coupled with flame ionization detection to simultaneously quantify the residual levels of ether,tetrahydrofuran,methanol,dichloromethane,ethanol,acetonitrile,pyridine and N,N-dimethylformamide in thymopentin.Methods A DB-WAX capillary column(30 m×0.32 mm× 1.00 μm)was utilized.The temperature program initiated at 40 ℃,held for 4 minutes,then ramped up at a rate of 10 ℃/min to 200 ℃ and maintained for 3 minutes.The injector temperature was 230 ℃.A flame ionization detector was employed,with the temperature at 250 ℃.High purity nitrogen gas served as the carrier gas,with a flow rate of 4mL/min.The injection method was split mode,with a split ratio of 10:1.The headspace vial equilibration temperature was 120℃,with an equilibration time of 30 minutes and a sample volume of 1.0mL.Results The method showed good linearity(r＞0.997)for the quantification of 8 different residual solvents within a certain concentration range.The quantitation limits for solvents above were 1.5,0.1,0.5,0.6,0.8,4.1,0.6 and 4.4 μg/mL.The average recovery rates were 92.9％,108.4％,106.0％,102.4％,107.5％,109.2％,107.8％and 91.2％,with RSD values were 4.1％,2.8％,1.0％,1.9％,1.1％,1.1％,0.6％和 1.7％,respectively.Conclusion The method is accurate and stable,and it can be used for the determination of 8 residual solvents in thymopentin for injection raw material.
万方数据
维普
