顶空气相色谱-硫化学发光检测器法测定药用胶塞中硫化剂及硫化促进剂  

Determination of Vulcanizing Agents and Accelerators in Pharmaceutical Rubber Stoppers by Headspace Gas Chromatography-Sulfur Chemiluminescence Detector

作　　者：辜倩 汪元亮 肖小武 赵霞[3] 朱碧君 朱必林 GU Qian;WANG Yuanliang;XIAO Xiaowu;ZHAO Xia;ZHU Bijun;ZHU Bilin(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,Nanchang 330029,China;Department of Pharmacy,Jiangxi University of Traditional Chinese Medicine,Nanchang 330004,China;National Institutes for Food and Drug Control,Beijing 100050,China;Jiangsu Institute of Medical Device Testing,Nanjing 210019,China)

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]江西中医药大学药学院,南昌330004 [3]中国食品药品检定研究院,北京100050 [4]江苏省医疗器械检验所,南京210019

出　　处：《医药导报》2025年第4期547-553,共7页Herald of Medicine

基　　金：江西省药品监督管理局科研项目资助(2021KY13);国家药典委标准提高课题(2019Y03)。

摘　　要：目的建立顶空气相色谱-硫化学发光检测器法(HS-GC-SCD)测定药用胶塞中9种硫化剂及硫化促进剂。方法采用DB-1毛细管柱(30 m×0.32 mm×0.25μm),以氦气为载气。进样口温度220℃,分流比10∶1,载气流速1.5 mL·min^(-1)。程序升温:初始温度设定为40℃·min^(-1),随后以5℃·min^(-1)的速度升高,直到达到60℃·min^(-1);随后,再以15℃·min^(-1)的速度升温,直至温度升至260℃·min^(-1)。SCD检测器参数:底座温度280℃,燃烧室温度800℃,空气流速为60 mL·min^(-1),氢气流速为40 mL·min^(-1)。结果样品前处理方法简单便捷,有效减少提取损失。方法学结果显示,在浓度范围内所有硫化物均表现出良好的线性关系(r^(2)≥0.990);精密度和重复性的相对标准偏差(RSD)均低于2%。平均回收率范围86.4%~97.5%。通过对样品检测结果的分析,发现胶塞中普遍存在游离硫。结论该方法操作简单,与其他现有检测方法相比,HS-GC-SCD的基质效应更小,灵敏度和选择性更高,适用于不同药用胶塞中硫化剂和硫化促进剂的含量测定。Objective The aim of this study was to develop a method for the determination of nine vulcanizing agents and accelerators in pharmaceutical rubber stoppers by headspace gas chromatography with sulfur chemiluminescence detector(HS-GC-SCD).Methods A DB-1 capillary column(30 m×0.32 mm×0.25μm)was used with He as the carrier gas.The injection port temperature was 220℃,the split ratio was 10∶1,and the carrier gas flow rate was 1.5 mL·min^(-1).The temperature program was as follows:the starting temperature was 40℃,and it was increased to 60℃at a rate of 5℃per minute,and then to 260℃at a rate of 15℃per minute.SCD detector parameters:base temperature was 280℃,combustion chamber temperature was 800℃,air flow rate was 60 mL·min^(-1),and hydrogen flow rate was 40 mL·min^(-1).Results The sample pretreatment method was simple and convenient,and it effectively reduced the extraction loss.The methodological results showed that all sulfides showed good linear relationships within the concentration range(r^(2)≥0.990).The RSD was less than 2%;and the average recovery rate was 86.4%-97.5%.From the analysis of the sample test results,free sulfur is commonly found in rubber stoppers.Among all the samples of the vulcanization system,the free sulfur detected in the sulfur vulcanization system is higher than the free sulfur produced by degradation of other vulcanization systems.Conclusions This method is simple to operate,compared with other existing detection methods.HS-GC-SCD has a smaller matrix effect,higher sensitivity and selectivity,and is appropriate for quantifying the concentrations of sulfide present in various rubber stoppers.

关 键 词：药用胶塞 硫化学发光检测器 硫化剂 硫化促进剂 

分 类 号：R0657.63[医药卫生]