GC法测定盐酸司他斯汀中2-氯乙醇基因毒性杂质  

Determination of 2-Chloroethanol as a Genotoxic Impurity in Setastine Hydrochloride by GC

作　　者：夏红英 温雯 钟振华 刘贞 余师师 裴昆 刘荷英 程奇珍 Xia Hongying;Wen Wen;Zhong Zhenhua;Liu Zhen;Yu Shishi;Pei Kun;Liu Heying;Cheng Qizhen(Jiangxi Institute for Drug Control,NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine,Jiangxi Province Engineering Research Center for Drug and Medical Device Quality,Nanchang 330029,China;Jiangxi Center for Drug Certification and Evaluation,Jiangxi Center for Medical Device Evaluation)

机构地区：[1]江西省药品检验检测研究院国家药品监督管理局中成药质量评价重点实验室江西省药品与医疗器械质量工程技术研究中心,南昌330029 [2]江西省药品认证审评中心江西省医疗器械技术审评中心

出　　处：《中国药师》2020年第12期2480-2482,共3页China Pharmacist

基　　金：江西省药品监督管理局科研项目(编号:2019JS06);国家药品标准提高研究项目[药典综[2018]482号,编号:2018H093]。

摘　　要：目的:建立气相色谱法测定盐酸司他斯汀中2-氯乙醇的残留量。方法:采用HP-5(60 m×0.320 mm,1.00μm)毛细管柱;以微池电子捕获检测器(u ECD)为检测器,温度为280℃;进样口温度为220℃;柱温:程序升温,起始温度为40℃,维持13 min,以50℃·min-1的速率升温至310℃,维持10 min;载气为氮气,流速为4.0 ml·min-1;分流比:3∶1,进样量为1μl。结果:2-氯乙醇在2.038~13.250μg·ml-1浓度范围内,线性关系良好(r=0.9978),平均回收率为85.90%,RSD=2.41%(n=9),定量限为1.019μg·ml-1(0.0025%),检测限为0.510μg·ml-1(0.0013%)。结论:本测定方法操作简便、准确、经济,可用于盐酸司他斯汀原料药中2-氯乙醇残留量的日常检测。Objective: To establish a capillary GC method for the determination of 2-chloroethanol in setastine hydrochloride.Methods: The capillary column GC was used with an HP-5 capillary column( 60 m×0.320 mm,1.00 μm). u ECD was used as the detector with the temperature at 280℃.The injector temperature was 220℃,and the column temperature was raised by programming: the initial temperature was 40℃,maintained for 13 min,and then rose to 310℃ at the rate of 50℃·min-1,and maintained for 10 min.The flow rate of carrier gas N2 was 4.0 ml·min-1. The split ratio was 3 ∶ 1,and the injection volume was 1 μl. Results: The linearity of 2-chloroethanol was good within the experimental concentration range( 2.038-13.250μg· ml-1,r = 0.997 8). The average recovery was 85.9%( RSD = 2. 41%,n = 9). The limit of quantification was 1. 019μg·ml-1( 0.002 5%),and the limit of detection was 0.510μg·ml-1( 0.001 3%). Conclusion: The method is simple,accurate and economical,which can be used for the routine determination of residual 2-chloroethanol in setastine hydrochloride.

关 键 词：盐酸司他斯汀 2-氯乙醇 基因毒性杂质 气相色谱法 

分 类 号：R927.1[医药卫生—药学]