第 50 卷第 3 期 Vol. 50 No. 3 2020 年 6 月 Jun 2020

所属栏目：分析与测试 顶空气相色谱法测定异丁司特原料药中有机溶剂的残留量

付丙月1，崔新强1，吴伟山2，王金虎1* （1. 山东省药学科学院 山东省化学药物重点实验室，山东 济南 250101；2. 山东省中医药大学 附属医院骨科，山东 济南 250011）

摘　要：以Agilent DB-624毛细管柱为色谱柱，程序升温，氢火焰离子化检测器，采用顶空气相色谱法。建立同时测定异丁司特原料药中乙醇、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、甲苯六种有机溶剂残留量的方法。在此色谱条件下，乙醇、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、甲苯这六种待测有机残留溶剂的分离度均大于1.5，空白溶剂无干扰，线性、准确度、精密度良好。该方法操作简单，重复性好，适用于异丁司特原料药中六种有机溶剂残留的同时测定。

关键词：异丁司特；气相色谱法；顶空进样；有机溶剂残留

中图分类号：O657.7　　文献标识码：A　　文章编号：1009-9212（2020）03-0069-04

Determination of Organic Solvent Residual in Ibudilast by Headspace Gas Chromatography

FU Bing-yue1, CUI Xin-qiang1, WU Wei-shan2, WANG Jin-hu1* (1. Shandong Provincial Key Laboratory of Chemical Drugs Shandong Academy of Pharmaceutical Sciences, Jinan 250101, China; 2. Affiliated Hospital of Shandong University of Traditional Chinese Medicine Department of Orthopedics, Jinan 250011, China)

Abstract：In this headspace gas chromatography method, the Agilent DB-624 capillary column was used as the chromatographic column, the temperature was programmed and the hydrogen flame ionization detector was used. To establish a method for the simultaneous determination of the residuals of six kinds of organic solvents including ethanol, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran, and toluene in Ibudilast. Under this chromatographic condition, the resolution of the organic solvents including ethanol, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran, and toluene were all greater than 1.5, while the blank solvent had no interference, and the linearity, accuracy, and precision were good. This method was proved to be simple, repeatable, and suitable for the simultaneous determination of 6 organic solvent residues in Ibudilast.

Key words：ibudilast; gas chromatography; headspace sampling; residual organic solvents

基金项目：山东省重大科技创新工程项目（2019JZZY010520）。

作者简介：付丙月（1985-），女，山东济南人，硕士，主要从事新药研发和药物分析（E-mail：fubingyue-2004@163.com）。

联 系 人：王金虎，副主任药师，主要从事药物分析（E-mail：wjh1573@126.com）。

收稿日期：2020-05-21