QuEChERS-UPLC法测定化妆品中10种性激素

Determination of 10 sex hormones in cosmetics by QuEChERS-UPLC

建立了QuEChERS-UPLC法测定化妆品中10种性激素的方法。样品利用饱和氯化钠进行分散,乙腈超声提取后经QuEChERS净化。采用CORTECS C_(18)+(2.1 mm×100 mm,2.7μm)色谱柱分离,以乙腈-水为流动相进行梯度洗脱,PDA检测器多波长检测,外标法定量。结果表明,10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0.02~0.1μg/mL和0.05~0.3μg/mL。在5,25和50μg/g 3个加标水平下的回收率为81.2%~103.5%,相对标准偏差(RSD,n=6)为0.5%~12.0%。该方法操作简便、重现性好,适用于化妆品中性激素的测定。

A method of QuEChERS coupled with ultra-high performance liquid chromatography was developed for determination of 10 sex hormones in cosmetics.The sample was dispersed using saturated sodium chloride,and purified by QuEChERS after acetonitrile ultrasound extraction.Chromatographic separation was achieved on a CORTECS C_(18)+column(2.1 mm×100 mm,2.7μm)by gradient elution using acetonitrile-water as mobile phase.PDA detector was used to test samples at multiple wavelengths,and external standard method was used for quantification.Results show that there is a good linear relationship for each of the 10 sex hormones in respective mass concentration range with their correlation coefficients(r)all above 0.99.The limits of detection(LOD)and the limits of quantitation(LOQ)for the 10 sex hormones are in the range of 0.02-0.1μg/mL and 0.05-0.3μg/mL,respectively.Average recoveries at three levels of 5,25 and 50μg/g are in the range of 81.2%-103.5%,with relative standard deviations(RSD,n=6)of 0.5%-12.0%.With the advantages of simplicity and good reproducibility,this method is suitable for the analysis of sex hormones in cosmetics.