气相色谱-质谱法测定化妆品中的丙烯腈  

Determination of Acrylonitrile in Cosmetics by GC-MS Method

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：《分析测试学报》2011年第1期81-84,共4页Journal of Instrumental Analysis

摘　　要：建立了化妆品中丙烯腈的气相色谱-质谱分析方法。不同类型的化妆品样品中加入甲醇超声提取，经高速离心处理浓缩后，采用OasisHLB固相萃取柱净化，1mL20％甲醇溶液淋洗，3mL80％甲醇溶液洗脱，收集洗脱液，浓缩后经无水疏酸钠脱水，进行气相色谱-质谱定性及定量分析。选用HP—INNOWax（60m×0．25mm×0．50μm）石英毛细管柱，流速1．2ml/min，采用电子轰击电离源，选择监测离子m／z53、52、26（其中53为定量离子），外标法定量。方法的平均回收率为84％-101％，相对标准偏差（RSD）为1．1％～4．2％，对丙烯腈的检出限为0．4mg/kg。该方法快速、准确、灵敏度高，可用于化妆品中丙烯腈的测定。A gas chromatography - mass spectrometric method was developed for the determination of acrylonitrile in cosmetic samples. The cosmetics were ultrasonically extracted with methanol and then centrifuged. The concentrated supernatant was purified with an Oasis HLB solid phase extraction cartridge using 20% methanol solution as washing agent and 80% methanol solution as eluting agent. The eluent was further dehydrated with anhydrous sodium sulphate. The analysis was carried out with a capillary column（ HP-INNOWax 60 m×0.25 mm×0. 50 μm） under electron ionization conditions at a flow rate of 1.2 mL/min. The quantitation was performed by the external standard method under selected ion monitoring （SIM） mode using monitering ions of rn/z 53, 52 and 26. The recoveries were in the range of 84% -101% with relative standard deviations（RSDs） of 1.1% -4. 2%. The detection limit was 0. 4 mg/kg. This method was proved to be simple, accurate, and was suitable for the determination of acrylonitrile in cosmetics.

关 键 词：化妆品 丙烯腈 固相萃取 气相色谱-质谱法 

分 类 号：O657.71[理学—分析化学] S482.294[理学—化学]