固相萃取-超高效液相色谱串联质谱法测定化妆品中国标方法以外的42种糖皮质激素

Determination of 42 glucocorticoids beyond the national standard method in cosmetics by solid phase extraction-liquid chromatography tandem mass spectrometry

建立了针对化妆品中多种糖皮质激素的固相萃取-超高效液相色谱串联质谱检测法,除了可对化妆品中已有检测标准的50种糖皮质激素实现检测外,还可实现国标以外的42种糖皮质激素检测。样品经分散、提取及净化后,选用UPLC Shim-pack XR-ODSⅢC_(18)(2.0 mm×150 mm,2.2μm)的色谱柱,以0.1%(V/V)乙酸乙腈溶液和0.1%(V/V)乙酸水溶液为流动相,在电喷雾离子源(ESI)及多反应监测(MRM)模式下,对目前国标法以外的42种糖皮质激素进行同步测试。42种糖皮质激素均呈现良好线性响应,相关系数达到0.99以上。针对水剂、乳液、霜类基质样品,采用加标回收法测试,检出限可达0.03μg/g,定量限可达0.1μg/g,三基质三水平六平行试验的平均回收率在67.6%~112.5%范围内。采用所建立的方法,已筛查出实际样本中添加了这42种糖皮质激素成分的阳性样品2个。以固相萃取-超高效液相色谱串联质谱法测定可为监测化妆品中糖皮质激素的非法添加提供更为高效检测途径和方法。

A solid phase extraction(SPE)-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was developed for the determination of 42 glucocorticoids in cosmetics,in addition to the existing standard of 50 glucocorticoids.After the samples were dispersed,extracted and purified,42 glucocorticoids were determined by using UPLC Shim-pack XR-ODSIII C_(18)(2.0 mm×150 mm,2.2μm)chromatographic column,0.1%(V/V)acetic acid acetonitrile solution and 0.1%(V/V)acetic acid aqueous solution as the mobile phase at the mode of electrospray ionization(ESI)and multiple reaction monitoring(MRM).A total of 42 hormones have good linearity,and the correlation coefficients are above 0.99.For water,emulsion and cream substrates,the limit of detection(LOD)is 0.03μg/g and the limit of quantification(LOQ)is 0.1μg/g.The average recoveries of three levels and six parallel tests range from 67.6%-112.5%for water,emulsion and cream substrates.At present,two positive samples with these 42 glucocorticoid components have been screened,which provides a more comprehensive method for monitoring the illegal addition of glucocorticoids in cosmetics.