稳定同位素稀释气相色谱-质谱联用测定化妆品中5种磷酸三酯类化合物

Determination of Organophosphate Esters in Cosmetics by Stable Isotope Dilution-Gas Chromatography-Mass Spectrometry

根据不同化妆品的基质特性探讨优化不同的提取净化方法,建立了稳定同位素稀释气相色谱-质谱联用测定化妆品中5种磷酸三酯类化合物（ OPEs）的方法。膏霜乳液类和蜡基类化妆品经溶剂提取后,采用ENVI-Carb固相萃取柱净化；粉剂类和水剂类化妆品经溶剂提取、浓缩后直接检测。样液经DB-5MS（30 m×0.25 mm×0.25μm）色谱柱分离,GC-MS的选择离子监测（ SIM）模式检测,以保留时间和特征离子丰度比定性,稳定同位素稀释内标法定量。在优化的实验条件下,5种磷酸三酯类化合物在各自的线性范围内相关系数大于0.9995,方法检出限为1.0～30μg/kg,平均回收率为89.5%～105%,相对标准偏差（n=6）为2.9%～9.1%。本方法净化效果好,可有效消除基质效应,且有较好的回收率,可用于不同类型的化妆品基质中磷酸三酯类化合物的测定。

A method based on stable isotope dilution gas chromatography-mass spectrometry （ GC-MS ） was established to determine five kinds of organophosphate esters （ OPEs ） in different kinds of cosmetics. For cream and wax-based cosmetics, samples were extracted by appropriate solvent, and then purified by ENVI-Carb solid phase extracting column. For powder and aqueous samples, GC-MS test could be operated directly after solvent extraction and concentration. All of the samples were separated by DB-5MS （30 m×0. 25 mm× 0. 25 μm） chromatographic column, and detected by selected ion monitoring （ SIM ） mode. The target analytes were qualitatively confirmed by retention time and abundance ratio of characteristic ions, and quantified by stable isotope diluted internal standard method. Under the optimized conditions, the linear coefficients of the OPEs were larger than 0. 9995, the detection limits were 1. 0-30 μg/kg, the average recoveries （ n=6 ） ranged from 89 . 5% to 105%, and the RSDs were in the range of 2 . 9%-9 . 1%. The developed method, which was characteristic by satisfactory purification effect, favorable matrix effect elimination capacity, as well as high recovery, was suitable for the determination of OPEs in different kinds of cosmetic matrices.