本文關(guān)鍵詞： 氣相色譜電子捕獲法 藥品 氯代乙烷類化合物　出處：《中國新藥雜志》2017年21期 　論文類型：期刊論文

【摘要】：目的:建立氣相色譜法同時測定藥品中氯代乙烷類毒性雜質(zhì)的分析方法。方法:采用氣相色譜法,電子捕獲檢測器(ECD),DB 624(30 m×0.53 mm,3.0μm)毛細(xì)管色譜柱,程序升溫,采用外標(biāo)法定量。結(jié)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)范圍內(nèi)線性關(guān)系良好,線性相關(guān)系數(shù)均大于0.999。平均回收率在94.0%~102.0%,RSD為1.5%~4.4%,檢出限分別為26.03,5.510,0.031 25,1.027 8,0.050 00和0.258 5 ng·m L~(-1)。結(jié)論:所建立的氣相色譜法能夠快速、準(zhǔn)確、靈敏的檢測藥品中氯代乙烷類雜質(zhì)的含量,為藥品的質(zhì)量評價提供依據(jù)。
[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.
【作者單位】： 北京協(xié)和醫(yī)學(xué)院中國醫(yī)學(xué)科學(xué)院藥物研究所;
【基金】：國家“重大新藥創(chuàng)制”科技重大專項資助項目(2012ZX09301002-001-006) 協(xié)和創(chuàng)新團(tuán)隊項目-藥物藥效和安全性相關(guān)的關(guān)鍵分析新技術(shù)研究資助項目(2016-I2M-3-010)
【分類號】：O657.71;R927.1
【正文快照】： 與普通雜質(zhì)相比,致癌性雜質(zhì)(包括遺傳毒性致癌物和非遺傳毒性致癌物),特別是遺傳毒性雜質(zhì)的安全閾值較低[1]。自2002年起,歐洲藥品管理局(EMA)[2]、美國食品藥品監(jiān)督管理局(FDA)[3]以及人用藥品注冊技術(shù)要求國際協(xié)調(diào)會議(ICH)[4]先后發(fā)表了關(guān)于藥品中遺傳毒性雜質(zhì)的指導(dǎo)原則。

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