液相色谱-串联质谱法快速测定化妆品中的丙烯酰胺

Rapid determination of acrylamide in cosmetics by liquid chromatography-tandem mass spectrometry

建立了水基类、油基类、凝胶类、膏霜乳液类、粉类5类化妆品中丙烯酰胺的液相色谱-串联质谱快速测定方法,样品以水、石油醚（30℃~60℃）提取、离心后,水层加5%甲酸溶液、石油醚（30℃~60℃）,再涡旋、离心,取水相过滤,滤液采用Prodigy C18色谱柱（4.6 mm×150 mm,3.0μm）进行分离。流动相为甲醇和0.05%甲酸溶液,梯度洗脱。质谱测定采用多反应监测模式,监测离子为m/z 72.0→m/z 55.0,m/z 72.0→m/z 54.0,内标法定量。结果丙烯酰胺在0.03~2 mg/kg范围内,线性良好,回收率为90.2%~114.5%,RSD≤9.0%。方法可用于化妆品中丙烯酰胺的快速测定。

A method of liquid chromatography- tandem mass spectrometry（ LC-MS/MS） has been established for the rapid determination of acrylamide in 5 kinds of cosmetics,including water-based cosmetics,oil-based cosmetics,gel,cream and powder. Samples were extracted by water and petroleum ether（ 30 ~ 60 ℃）. The extractives were centrifuged. The water layer was separated and added with 5% formic acid solution and petroleum ether（ 30 ~ 60 ℃）. After vortex and centrifugation,the water layer was filtered. Ten microliter of filtrate was separated on a Prodigy C18column（ 4. 6 mm × 150 mm,3. 0 μm） with a gradient elution of methanol and 0. 05% formic acid solution. Acrylamide was detected by MRM mode with transitions of m/z 72. 0 →m/z 55. 0 and m/z 72. 0 → m/z 54. 0. The quantification was performed by using 2,3,3- D3 acrylamide as internal standard. A good linear relationship was obtained in the range of 0. 03 ~ 2 mg/kg. The recoveries of acrylamide at different spiked levels were 90. 2% ~ 114. 5% with the RSDs ≤ 9. 0%. The method is simple,sensitive,specific and rapid.