同位素稀释液相色谱-串联质谱法测定化妆品中残留的丙烯酰胺

建立了化妆品中丙烯酰胺残留的同位素稀释液相色谱-串联质谱的分析方法。水溶性化妆品样品以水为提取溶剂进行提取,提取液经高速离心处理后,上清液用Oasis HLB固相萃取柱净化;脂溶性化妆品样品以正己烷和水混合溶剂液-液分配萃取。经Waters Atlantis T3色谱柱(150 mm×2.1 mm,3 μm)分离后在多反应监测模式下进行串联质谱定性及定量分析,以13C3-丙烯酰胺为内标定量。方法的定量限为0.1 mg/kg,在0.1～1.0 mg/kg 3个添加水平范围内的平均回收率为87.7%～95.8%,日内测定精密度均小于10%,日间测定精密度均小于12%。该方法能够满足化妆品中丙烯酰胺残留的检测要求。

Determination of acrylamide residue in cosmetics by isotope dilution-liquid chromatography-tandem mass spectrometry

A comprehensive analytical method based on isotope dilution-liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the determination of acrylam-ide residue in cosmetics. Water-soluble cosmetic sample was extracted with water, and the ex-tract was centrifuged, then the upper solution was cleaned up by an Oasis HLB solid phase ex-traction cartridge. Oil-soluble cosmetic sample was extracted by liquid-liquid partition with n-hexane and water. The qualitative and quantitative analyses were carried out for the analyte in the multiple reaction monitoring (MRM) mode after the chromatographic separation on a Wa-ters Atlantis T3 column (150 mm × 2. 1 mm, 3 μm). The quantification was performed with ~(13)C_3-acrylamide as internal standard. The limit of quantification (LOQ) for acrylamide was 0. 1 mg/kg. The mean recoveries were 87. 7% -95. 8% at the spiked levels of 0.1-1.0 mg/kg with the intra-day precision less than 10% and the inter-day precision less than 12%. The method is suitable for the determination of acrylamide in cosmetics.