UPLC-MS/MS法测定油基类化妆品中39种性激素

Determination of 39 sex hormones in oil-based cosmetics by ultra-performance liquid chromatography-tandem mass spectrometry

建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定油基类化妆品中39种性激素的方法。样品经正己烷分散,70%乙腈超声提取,在CORTECS C;(2.1 mm×150 mm,2.7μm)色谱柱上分离,流动相为乙腈-水进行梯度洗脱,采用多反应监测(MRM)模式测定。结果表明,39种性激素在该方法下的基质效应值为0.78~1.26,检出限(LODs)和定量限(LOQs)分别为0.6~2.3μg/L和1.9~6.8μg/L,在1.87~67.41μg/L范围内线性关系良好(相关系数r>0.995)。在0.25,0.50和1.00μg/g 3个加标水平下的回收率为81.7%~110.6%,相对标准偏差(RSD,n=6)为1.2%~14.1%。该方法前处理简便,准确性好,适用于油基类化妆品中性激素的测定。

An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of39 sex hormones in oil-based cosmetics.The sample was dispersed with n-hexane,then extracted with 70%acetonitrile,and separated on a CORTECS C;(2.1 mm×150 mm,2.7μm) column by gradient elution using acetonitrile-water as mobile phase.The analysis was performed under multiple reaction monitoring (MRM) mode.The results showed that the matrix effects of 39 sex hormones were 0.78-1.26.The limits of detection (LODs) and limits of quantitation (LOQs) for 39 sex hormones were in the range of 0.6-2.3μg/L and 1.9~6.8μg/L,respectively.There was good linear relationship for 39 sex hormones in the mass concentration range of 1.87-67.41μg/L with their correlation coefficients (r) all above 0.995.The average recoveries at three spiked levels of 0.25,0.50 and 1.00μg/g were in the range of 81.7%-110.6%,with relative standard deviations (RSDs,n=6) of 1.2%-14.1%.The simplicity and accuracy of this method make it suitable for the analysis of sex hormones in oil-based cosmetics.