GC-MS法测定盐酸西替利嗪中的2个烷基氯代物杂质
Determination of Two Alkyl Chlorides in Cetirizine Dihydrochloride by Gas Chromatography-mass Spectrometry
韩忠丽 1卢红华 1李婷 1郝贵周 1张贵民1
作者信息
- 1. 鲁南制药集团股份有限公司,国家手性制药工程技术研究中心,山东临沂 273400
- 折叠
摘要
建立了气相色谱-质谱法测定盐酸西替利嗪(1)中的遗传毒性杂质4-氯-4-甲基戊烷-2-酮(2)和2,6-二氯-2,6-二甲基庚烷-4-酮(3).采用VF-WAXms毛细管柱(0.25 mm×30 m×0.25 μm),选择离子监测模式进行测定.结果显示,2和3分别在75.86～455.16、75.18～451.08 ng/mL内线性关系良好,定量限分别为0.025和0.066 ng/mL,回收率分别为101.66％、102.46％.建立的方法可测定1中的2和3,为1的质量研究提供了参考.
Abstract
A gas chromatography-mass spectrometry(GC-MS)method was established for two genotoxic alkyl chloride impurities,namely 4-chloro-4-methylpentan-2-one(2)and 2,6-dichloro-2,6-dimethyl-4-heptanone(3),in cetirizine dihydrochloride(1).The VF-WAXms capillary column(0.25 mm×30 m×0.25 μm)was used,and the measurement was performed in selected ion monitoring(SIM)mode.The results showed that it was linear for 2 and 3 in the ranges of 75.86-455.16 ng/mL and 75.18-451.08 ng/mL.The limits of quantification were 0.025 and 0.066 ng/mL,respectively.Tthe recoveries were 101.66％and 102.46％,respectively.The established method can determine 2 and 3 in 1,which provide a reference for the quality study of 1.
关键词
气相色谱-质谱法/盐酸西替利嗪/4-氯-4-甲基戊烷-2-酮/2,6-二氯-2,6-二甲基庚烷-4-酮/基因毒性杂质Key words
gas chromatography-mass spectrometry/cetirizine dihydrochloride/4-chloro-4-methylpentan-2-one/2,6-dichloro-2,6-dimethyl-4-heptanone/genotoxic impurity引用本文复制引用
出版年
2024
NETL
NSTL
万方数据