超高效液相色谱-串联质谱法同时测定化妆品中35种性激素

Simultaneous Determination of 35 Sex Hormones in Cosmetics by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry

采用超高效液相色谱-串联质谱(UPLC-MS/MS)建立了同时测定化妆品中35种性激素的方法。样品经50%乙腈水溶液超声提取,采用CORTECS C18(2.1 mm×150 mm,2.7μm)色谱柱分离,以乙腈-水为流动相进行梯度洗脱,多反应监测(MRM)模式测定。结果表明,35种性激素在各自的质量浓度范围内线性关系良好(相关系数r>0.99),检出限(LOD)和定量下限(LOQ)分别为0.028~0.117μg/g和0.093~0.352μg/g。在0.25、0.50、1.00μg/g 3个加标水平下,水状、乳状和霜状3种基质样品的回收率为84.0%~117%,相对标准偏差(RSD,n=6)为1.5%~14%。该方法前处理简单、灵敏度高、准确性好,适用于化妆品中性激素的测定。

An ultra-performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the simultaneous determination of 35 sex hormones in cosmetics.The sample was ultrasonically extracted with 50% acetonitrile solution,and separated on a CORTECS C18(2.1 mm×150 mm,2.7 μm) column by gradient elution using acetonitrile-water as mobile phases.The analysis was performed under multiple reaction monitoring(MRM) mode. Results showed that there were good linear relationships for 35 sex hormones in the respective concentration range with their correlation coefficients(r) all above 0.99.The limits of detection(LOD) and limits of quantitation(LOQ) for 35 sex hormones were in the ranges of 0.028-0.117 μg/g and 0.093-0.352 μg/g,respectively.Average recoveries of toner,emulsion and cream samples at three levels of 0.25,0.50,1.00 μg/g were in the range of 84.0%-117%,with relative standard deviations(RSD,n=6) of 1.5%-14%.With the advantages of simplicity,sensitivity and accuracy,this method is suitable for the analysis of sex hormones in cosmetics.