气相色谱-质谱法测定化妆品中的三氯叔丁醇  

Determination of chlorobutanol in cosmetics by gas chromatography-mass spectrometry

作　　者：刘茜[1] 马强[1] 席海为[1] 王烨[1] 白桦[1] 王超[1] 

机构地区：[1]中国检验检疫科学研究院,北京100123

出　　处：《分析试验室》2011年第9期55-58,共4页Chinese Journal of Analysis Laboratory

基　　金：质检公益性行业科研专项计划项目(200910267);国家标准委员会计划项目(20090926-T-607)资助

摘　　要：建立了测定化妆品中三氯叔丁醇的气相色谱-质谱分析方法。膏霜、水剂、散粉、香波、唇膏等不同类型的化妆品样品加入50%甲醇-无水乙醇或无水乙醇超声提取后,样品提取液高速离心处理,取上清液经无水硫酸钠脱水,进行气相色谱-质谱定性及定量分析。选用DB-1701(30 m×0.25 mm×0.25μm)石英毛细管柱,程序升温,流速1.0 mL/min,采用电子轰击电离源,选择监测离子(m/z 53、59、125,其中59为定量离子),外标法定量。方法的平均回收率为83.4%～107.6%,相对标准偏差(RSD)为1.0%～5.3%,膏霜、水剂、散粉、香波、唇膏等不同类型化妆品中二氯叔丁醇的检出限均为0.8 mg/kg。A gas chromatography-mass spectrometric method was developed for the determination of chlorobutanol in cosmetic samples.The cream,lotion,powder,shampoo and lipstick samples were ultrasonically extracted with 50% methanol-ethanol or ethanol,and then centrifuged.The eluent was further dehydrated and then analyzed with a capillary column（DB-1701,30 m × 0.25 mm × 0.25 μm） under electron ionization conditions at a flow rate of 1.0 mL/min.The quantitation was performed by the external standard method under selected ion monitoring mode（SIM） using monitoring ions of m/z 53,59,125.The recoveries were 83.4%~107.6%,with the relative standard deviations（RSDs） of 1.0%~5.3%.All the detection limit of cream,lotion,powder,shampoo and lipstick samples was 0.8 mg/kg.This method was proved to be simple,accurate,and stable by testing experiments,which was suitable for the detection of chlorobutanol in cosmetics.

关 键 词：气相色谱-质谱 化妆品 三氯叔丁醇 

分 类 号：O657.63[理学—分析化学]