顶空气相色谱法测定明胶空心胶囊中EO和ECH的残留量  

Determination of EO and ECH Residual Solvents in Vacant Gelatin Capsules by Headspace Caplillary GC

作　　者：周云婷 杨慧萍 钱菁 吕泽斌 章媛媛 倪慧慧 ZHOU Yun-ting;YANG Hui-ping;QIAN Jing;LYU Ze-bin;ZHANG Yuan-yuan;NI Hui-hui(Xinchang Food and Drug Inspection and Testing Center,Xinchang 312500,China)

机构地区：[1]新昌县食品药品检验检测中心,浙江新昌312500

出　　处：《化工管理》2022年第13期47-50,共4页Chemical Engineering Management

基　　金：绍兴市市场监督管理局2021年度市级市场监管系统课题攻关计划项目(2021-23)。

摘　　要：文章建立了同时测定明胶空心胶囊中环氧乙烷、氯乙醇残留量的质量控制方法。采用6%氰丙基苯基-94%二甲基硅氧烷为固定液的毛细管柱为色谱柱,氢火焰离子化检测器(FID),载气为氮气;进样口温度为200℃,检测器温度为250℃。顶空进样,顶空平衡温度90℃,进样量为3mL。环氧乙烷的检测限、定量限分别为0.03μg/mL和0.1μg/mL,氯乙醇的检测限、定量限分别为0.6μg/mL和2μg/mL;环氧乙烷在0.1~10μg/mL浓度范围内线性关系良好(r=1.0000),氯乙醇在2~200μg/mL浓度范围内线性关系良好(r=1.0000);精密度结果中环氧乙烷含量、氯乙醇含量的RSD均小于2%;初始柱温、炉温、平衡时间发生较小变动对检测环氧乙烷含量、氯乙醇含量几乎没有影响。该方法前处理简单,色谱方法专属性强、检测灵敏度高、精密度良好、环氧乙烷和氯乙醇在各自的浓度范围内线性关系良好,可用于明胶空心胶囊中环氧乙烷和氯乙醇残留量的同时控制。In this paper,a method for determination of ethylene oxide(EO)and ethylene chlorohydrin(ECH)residual solvents in Vacant Gelatin Capsules was established.The method was performed on the capillary column with stationary phase was 6%cyanopropyl phenyl-94%dimethyl siloxane,the detector was FID,the carried gas was nitrogen.The inlet temperature was 200℃and FID detector temperature was 250℃.Headspace conditions was as follows:the balance temperature for sample was 90℃and the sample volume was 3 mL.The LOD and LOQ of EO was 0.03μg/mL and 0.1μg/mL.The LOD and LOQ of ECH was 0.6μg/mL and 2μg/mL.EO was observed a good linearity over the range of 0.1-10μg/mL(r=1.0000)and ECH was observed a good linearity over the range of 2-200μg/mL(r=1.0000).The RSD of EO and ECH in precision test were both less than 2%.The content of EO and ECH remained stable when the conditions were changed such as initial column temperature,oven temperature and equilibrium time.The method was easy to use,had a high accuracy and good reproducibility.This method can be used to simultaneously determine the content of ethylene oxide(EO)and ethylene chlorohydrin(ECH)residual solvents in vacant gelatin capsules.

关 键 词：环氧乙烷 氯乙醇 明胶空心胶囊 顶空进样 

分 类 号：O62[理学—有机化学]