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Oasis HLB固相萃取柱净化,1 mL 20%甲醇溶液淋洗,3 mL 80%甲醇溶液洗脱,收集洗脱液,浓缩后经无水硫酸钠脱水,进行气相色谱-质谱定性及定量分析。选用HP INNOWax(60 m×025 mm × 050 μm)石英毛细管柱,流速12 mL/min,采用电子轰击电离源,选择监测离子m/z 53、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11%~42%,对丙烯腈的检出限为04 mg/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。
Abstract
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×025 mm×050 μm) under electron ionization conditions at a flow rate of 12 mL/min.The quantitation was performed by the external standard method under selected ion monitoring(SIM) mode using monitering ions of m/z 53,52 and 26.The recoveries were in the range of 84%-101% with relative standard deviations(RSDs) of 11%-42%.The detection limit was 04 mg/kg.This method was proved to be simple,accurate,and was suitable for the determination of acrylonitrile in cosmetics.
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