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.
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)
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)。
关键词
环氧乙烷
氯乙醇
明胶空心胶囊
顶空进样
ethylene oxide(EO)
ethylene chlorohydrin(ECH)
vacant gelatin capsule
headspace injection
