GC-SCD法测定药用胶塞中5种常用硫化促进剂  

Determination of Five Vulcanization Accelerators in Pharmaceutical Rubber Plugs by GC-SCD

作　　者：汪元亮 辜倩 朱碧君 饶艳春 常亮 Wang Yuanliang;Gu Qian;Zhu Bijun;Rao Yanchun;Chang Liang(Jiangxi Institute for Drug Control,NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine,Jiangxi Province Engineering Research Center of Drug and Medical Device Quality,Jiangxi,330029;Jiangxi University of Traditional Chinese Medicine,Jiangxi,330004)

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,江西330029 [2]江西中医药大学,江西330004

出　　处：《当代化工研究》2024年第18期74-76,共3页Modern Chemical Research

基　　金：江西省药品监督管理局科研项目“注射用卤化丁基橡胶塞中硫化物的分析检测方法研究”(项目编号:2021KY13)。

摘　　要：建立了药用胶塞中噻唑、4,4'-二硫代二吗啉、N-叔丁基-2-苯并噻唑次磺酰胺、一硫化四甲基秋兰姆、N-环己基-2-苯并噻唑次磺酰胺5种硫化促进剂的测定方法。样品经过甲醇超声后进入带有硫化学发光检测器(SCD)的气相色谱仪进行分析测定。结果表明:5种硫化物在0.5~50μg·mL^(-1)浓度范围内线性良好;相关系数r在0.9990~0.9999之间;平均回收率(n=9)在90.5%~111.4%之间,RSD在5.0%~6.8%之间,检测限在0.002~0.005 mg/g。本方法操作简便,专属性强,精密度好,可用于胶塞中5种硫化促进剂的分析检测。A method for the determination of five vulcanization accelerators in pharmaceutical rubber stoppers,including thiazole,4,4'-dithiodimorpholine,N-tert-butyl-2-benzothiazolesulfenamide,tetramethylthiuram monosulfide,and N-cyclohexyl-2-benzothiazolesulfenamide,was established.The samples were subjected to methanol ultrasound and then entered into a gas chromatograph with a sulfur chemiluminescence detector(SCD)for analysis and determination.The results showed that the five sulfides had good linearity in the concentration range of 0.5~50μg·mL^(-1);the cor-relation coefficient r is between 0.9990 and 0.9999.The average recovery rate(n=9)was between 90.5% and 111.4%,the RSD was between 5.0% and 6.8%,and the detection limit was between 0.002 mg/g and 0.005 mg/g.This method is simple to operate,has strong specificity and good precision,and can be used for the analysis and detection of five vulcanization accelerators in rubber stoppers.

关 键 词：硫化促进剂 硫化学发光检测器 胶塞 

分 类 号：O657.63[理学—分析化学]