化妆品中6种雌激素的液相色谱串联质谱检测方法研究

Determination of six kinds of estrogens in cosmetics by liquid chromatograph-tandem mass spectrometry

目的建立化妆品中六种雌激素的液相色谱串联质谱(LC-MS/MS)测定方法。方法分别优化选择合适的质谱及色谱条件,确定最佳分析条件。样品用甲醇溶解,涡流震荡,超声抽提,0.45μm滤膜过滤,采用LC-MS/MS测定。结果6种雌激素β-雌二醇(E2),雌三醇(E3),雌酮(E1),己烯雌酚(DES)和己烷雌酚(HE)的最低检出限(LOD)分别为2.4、0.2、0.7、12、6和5ng/g;最低定量限(LOQ)分别为8、0.7、2.4、40、20和17ng/g;6种雌激素在浓度(0～1000ng/mL)的范围内均呈现良好线性(相关系数≥0.9990),平均加标回收率在85.2%～102.8%之间,相对标准偏差均在2.76%～8.69%之间。测定市场抽检的28个样品,结果满意。结论该方法能在较短时间内同时检测化妆品中6种雌激素,灵敏度高,选择性好。

Objective To develop methods for the determination of six kinds of estrogens in cosmetics by Liquid Chromatograph-Tandem Mass Spectrometry（LC-MS /MS）.Methods Through choosing and optimizing experimental conditions,Methanol was chosen as the extracted solvent,super sonic extraction,then centrifuging,filtrating,and the filtrate was analysed by LC-MS /MS.Results Using this method,the LC-MS /MS response to these six estrogens was linear in the range 0 ～ 1000ng /ml.Level limit of detection of six estrogens were 2.4,0.2,0.7,12,6 and 5ng /g,respectively,and level limit of quantification of six estrogens were 8,0.7,2.4,40,20 and 17ng /g,respectively,the average spiking recovery rate was 85.2%-102.8%,and relative standard deviation（RSD） was within 2.76%-8.69%.28 cosmetics were sampled and analyzed and no estrogens were measured.Conclusion This method possesses fairly high sensitivity and good specificity.