超高效液相色谱-串联质谱法同时测定化妆品中13种性激素含量

摘要

An ultra-performance liquid chromatography-tandem mass spectrometric (UPLC-MS/ MS) method was established for the determination of thirteen sex hormones in cosmetics.Toner,oil,cream and mask cosmetic samples were extracted with 50％ acetonitrile by vortex,and separated on a C1s column.The analysis was performed under dynamics multiple reaction monitoring (DMRM) mode.The results showed that the limits of detection(LODs) for 13 sex hormones in various kinds of cosmetics were in the range of 0.001-0.026 μg/g.Good linear relationship existed between peak area and mass concentration of 0.89-64.80 μg/L with correlation coefficients higher than 0.995.The average recoveries were in the range of 80.8％-116.8％,with relative standard deviations(RS Ds,n =6) of 0.7％-14.4％.With the advantages of high efficiency,sensitivity and accuracy,this method fills the gaps of determining chlormadinone acetate and other sex hormones,and is suitable for the general detection of neutral sex hormones in cosmetics.%建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定化妆品中13种性激素含量的分析方法.液态水基类、液态油基类、膏霜乳液类(含面膜)化妆品采用50％乙腈超声提取,经C18色谱柱分离,采用动态多反应监测(DMRM)扫描方式测定.结果表明,13种性激素的检出限(LODs)为0.001 ～0.026 μg/g,在0.89 ～64.80 μg/L范围内线性关系良好,相关系数(r)均大于0.995.回收率为80.8％～ 116.8％,相对标准偏差(RSD,n=6)为0.7％～14.4％.该方法高效、灵敏、准确,填补了化妆品中醋酸氯地孕酮、己酸羟孕酮等化合物的测定方法空白,可作为化妆品中性激素类物质的通用检测方法,适用于多种基质化妆品中性激素的快速筛查.