气相色谱电子捕获法测定药品中氯代乙烷类毒性杂质

发布时间：2018-01-19 14:34

本文关键词： 气相色谱电子捕获法药品氯代乙烷类化合物　出处：《中国新药杂志》2017年21期 　论文类型：期刊论文

【摘要】：目的:建立气相色谱法同时测定药品中氯代乙烷类毒性杂质的分析方法。方法:采用气相色谱法,电子捕获检测器(ECD),DB 624(30 m×0.53 mm,3.0μm)毛细管色谱柱,程序升温,采用外标法定量。结果:1,1-二氯乙烷在0.104 1~10.41μg·m L~(-1),1,2-二氯乙烷在0.022 04~2.204μg·m L~(-1),1,1,1-三氯乙烷在0.123 4~4.935 ng·m L~(-1),1,1,2-三氯乙烷在5.105~510.5 ng·m L~(-1),1,1,1,2-四氯乙烷在0.400 0~20.00 ng·m L~(-1),1,1,2,2-四氯乙烷在2.068~41.36 ng·m L~(-1)范围内线性关系良好,线性相关系数均大于0.999。平均回收率在94.0%~102.0%,RSD为1.5%~4.4%,检出限分别为26.03,5.510,0.031 25,1.027 8,0.050 00和0.258 5 ng·m L~(-1)。结论:所建立的气相色谱法能够快速、准确、灵敏的检测药品中氯代乙烷类杂质的含量,为药品的质量评价提供依据。
[Abstract]:Objective: to establish a gas chromatographic method for the simultaneous determination of toxic impurities in chlorinated ethane. Methods: gas chromatography and electron capture detector (ECD) were used. DB624A30m 脳 0.53mm ~ (3.0 渭 m) capillary column, programmed temperature, quantitative analysis by external standard method. Results: 1. The concentration of 1-dichloroethane is 0.104 1U 10.41 渭 g 路mL ~ (-1) ~ (-1) ~ (-1) ~ (-1) -dichloroethane is 0.022 04 (2.204 渭 g 路m ~ (-1)) 渭 g 路m ~ (-1) 路L ~ (-1). The concentration of 1-trichloroethane was 0.123 4 ~ 4.935 ng 路m ~ (-1) ng 路mL ~ (-1) ~ (-1) ~ (-1) trichloroethane was 5.105 (510.5 ng 路m ~ (-1)), and that of trichloroethane was 0.123 4 ~ 4.935 ng 路m ~ (-1). The results showed that the concentration of TCE was 0.400 ng 路mL ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1). The linear range of 2-tetrachloroethane was in the range of 2.068 ~ 41.36 ng 路mL ~ (-1). The linear correlation coefficients were all greater than 0.999.The average recovery rate was 94.0 ~ 102.0 and the RSD was 1.5 and the detection limit was 26.03 ~ 5.510, respectively. Conclusion: the established gas chromatography is rapid and accurate. The content of chlorinated ethane impurities in drugs is determined sensitively, which provides basis for drug quality evaluation.
【作者单位】：北京协和医学院中国医学科学院药物研究所;
【基金】：国家“重大新药创制”科技重大专项资助项目(2012ZX09301002-001-006) 协和创新团队项目-药物药效和安全性相关的关键分析新技术研究资助项目(2016-I2M-3-010)
【分类号】：O657.71;R927.1
【正文快照】： 与普通杂质相比,致癌性杂质(包括遗传毒性致癌物和非遗传毒性致癌物),特别是遗传毒性杂质的安全阈值较低[1]。自2002年起,欧洲药品管理局(EMA)[2]、美国食品药品监督管理局(FDA)[3]以及人用药品注册技术要求国际协调会议(ICH)[4]先后发表了关于药品中遗传毒性杂质的指导原则。

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