化妆品中挥发性有机溶剂的通用检测方法

以化妆品配方中常见及禁用的36种有机溶剂为研究模板,建立了化妆品中挥发性有机溶剂残留评价初筛知识库、确证知识库和定量方法。初筛知识库包括双柱保留指数知识库和NIST质谱库。双柱保留指数知识库以保留指数为定性指标,选择极性的VF-1301ms和非极性的DB-5ms两根色谱柱,用顶空气相色谱-质谱法考察了36种有机溶剂在两种色谱分离系统中的保留特性。利用NIST MS search 2.0作为检索工具,同时建立了36种挥发性有机溶剂的顶空气相色谱-质谱定量方法。样品经60 ℃、30 min静态顶空后以连接了VF-1301ms石英毛细管色谱柱的气相色谱-质谱仪检测,外标法定量。方法检出限为0.01~3.3 μg/g,加标回收率为60.77%~126.60%。该方法从通用性的角度,为化妆品中挥发性有机溶剂残留的筛查、鉴别和定量提供方法,部分解决了测定化妆品中挥发性有机溶剂时需要针对不同检测目标建立不同方法以及潜在溶剂存在备选筛查的问题。

Generic method for determination of volatile organic solvents in cosmetics

A generic screening, confirmation and determination method was established based on 36 commonly used volatile organic solvents in cosmetics by headspace gas chromatography-mass spectrometry (GC-MS). This method included a database for pilot screening and identification of those solvents and their quantitative method. Pilot screening database was composed by two sections, one was household section built by two columns with opposite polarities (column VF-1301ms and DB-5ms) using retention index in different column systems as qualitative parameter, and the other was NIST MS search version 2.0. Meanwhile, the determination method of the 36 volatile solvents was developed with GC-MS. Cosmetic samples were dissolved in water and transferred to a headspace vial. After 30 min equilibration at 60 ℃, the samples were analyzed by GC-MS equipped with a capillary chromatographic column VF-1301ms. The external calibration was used for quantification. The limits of detection were from 0.01 to 3.3 μg/g, and the recoveries were from 60.77% to 126.6%. This study provided a generic method for pilot screening, identification, and quantitation of volatile organic solvents in cosmetics, and may solve the problem that different analytical methods need to be developed for different targeted compounds and pilot screening for potential candidate solvent residues.