气相色谱法测定达比加群酯中10种溶剂的残留-中国药事.pdf

中国药事 2017 年 3 月 第 31 卷 第 3 期 263 ·药物研究· 气相色谱法测定达比加群酯中 10 种溶剂的残留 1 2 2 2 1* （1. 延边大学，延吉 133000；2. 吉林省 张微 ，马长沙 ，黄晓光 ，段成军 ，马静洁 博大伟业制药有限公司，长春 130000） 摘要 目的： 建立气相色谱法检测达比加群酯中 10 种残留溶剂。方法： 以 Rtx-1 1.0μm）极性毛细管柱程序升温，以氮气为载气，FID 为检测器，进样口温度为 200 ℃，检测器温度为 250 ℃，对达比加群酯中 10 种残留溶剂（甲醇、乙醇、乙酸乙酯、丙酮、二氯甲烷、正己烷、四氢呋 喃、异辛烷、吡啶和甲苯）进行测定。结果：各残留溶剂组分均能被良好分离，各溶剂线性关系良好， 精密度 RSD 均不超过 3.50%，平均回收率为 96.0%~105.0%。结论：本文建立的方法可用于达比加群酯 中残留溶剂的测定。 关键词： 气相色谱法；达比加群酯；残留溶剂；甲醇；乙醇；乙酸乙酯；丙酮；二氯甲烷；正己烷； 四氢呋喃；异辛烷；吡啶；甲苯 中图分类号：R917 文献标识码：A 文章编号： 1002-7777(2017)03-0263-06 doi:10.16153/j.1002-7777.2017.03.006 Determination of Ten Solvent Residues in Dabigatran Etexilate by Gas Chromatography 1 2 2 2 1* Zhang Wei , Ma Changsha , Huang Xiaoguang , Duan Chengjun , Ma Jingjie (1. Yanbian University, Yanji 133000, China; 2. Jilin Province Broad Well Pharmaceutical Co., Ltd., Changchun 130000, China) Abstract Objective: To establish a gas chromatographic method for the determination of ten residual solvents in dabigatran etexilate. Methods: The Rtx-1 (60 m × 0.32 mm × 1.0 μm) polar capillary column was used to heat up the sample. Nitrogen was used as the carrier gas, FID was used as the detector, the inlet temperature was and the detector temperature was 250 ℃. Ten residual solvents (methanol, ethanol, ethyl acetate, acetone, dichloromethane, hexane, tetrahydrofuran, isooctane, pyridine and toluene) in picarbitol ester were quantified under the above conditions. Results: The residual solvents were well separated, the linear relationships were good, the RSDs were less than 3.50%, and the average recoveries were 96.0%-105.0%. Conclusion: The method demonstrated in this paper can be used for the determination of residual solvents in dabigatran etexilate. Keywords ： gas chromatography; dabigatran et