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.
维普
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