气相色谱法测定胸腺五肽原料药中残留溶剂  

Determination of Residual Solvents in Thymopentin Drug Substances by Gas Chromatography

作　　者：薛巧如[1] 冯楚 杨承勇[1] 陈华[1] XUE Qiaoru;FENG Chu;YANG Chenyong;CHEN Hua(Guangdong Institute for Drug Control,Guangzhou Guangdong 510663,China;Guangdong Medical University,Dongguang Guangdong 523109,China)

机构地区：[1]广东省药品检验所,广东广州510663 [2]广东医科大学,广东东莞523109

出　　处：《药品评价》2024年第6期677-680,共4页Drug Evaluation

基　　金：广东省药品检验所基金项目(SN2023004,SN2022003)。

摘　　要：目的 采用顶空气相色谱法同时测定胸腺五肽原料药中乙醚、四氢呋喃、甲醇、二氯甲烷、乙醇、乙腈、吡啶和N,N-二甲基甲酰胺等有机溶剂残留量。方法 采用DB-WAX(30 m×0.32 mm×1.00 μm);程序升温:初始温度40 ℃,维持4 min,以10 ℃/min的速率升温至200 ℃,维持3 min;进样口温度为230 ℃;检测器温度为250 ℃;载气为高纯氮气;流速为4 mL/min;分流模式,分流比为10∶1;顶空瓶平衡温度120 ℃;平衡时间为30 min;进样体积为1.0 mL。结果?8种检测残留溶剂在一定浓度范围内显示良好的线性(r>0.997),上述溶剂的定量限分别为1.5、0.1、0.5、0.6、0.8、4.1、0.6、4.4 μg/mL;回收率分别为92.9%、108.4%、106.0%、102.4%、107.5%、109.2%、107.8%和91.2%,RSD值分别为4.1%、2.8%、1.0%、1.9%、1.1%、1.1%、0.6%和1.7%。结论 本法准确、稳定、灵敏度高,可用于胸腺五肽原料药中8种残留溶剂的测定。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×1.00μm)was utilized.The temperature program initiated at 40°C,held for 4 minutes,then ramped up at a rate of 10°C/min to 200°C and maintained for 3 minutes.The injector temperature was 230°C.A flame ionization detector was employed,with the temperature at 250°C.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°C,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 4.4μg/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.

关 键 词：胸腺五肽 气相色谱法 残留溶剂 

分 类 号：R927.2[医药卫生—药学]