液质联用技术测定化妆品中二苯乙烯类激素

建立了一种利用液相色谱-串联质谱测定化妆品中己烷雌酚、双烯雌酚和己烯雌酚的方法。样品经固相萃取净化后,采用多反应监控(MRM)模式分析。通过比较实验结果,色谱柱选择为Phenomenex Luna C18柱;流动相为水和乙腈,流速为200μL.min-1;梯度洗脱:初始时水的体积分数占70%,保持4 min,4～7 min时水的体积分数由70%线性变为20%。在此条件下该3种二苯乙烯类激素的检出限均为0.125 ng.g-1,定量限均为0.25 ng.g-1;在添加水平为1.25和12.5 ng.g-1时,不同样品不同添加水平的回收率为87.5%～100.3%,相对标准偏差为2.9%～4.7%(n=15)。

Determination of stilbene series hormone in cosmetics by HPLC-MS technology

A method using high performance liquid chromatography-mass spectrometry(HPLC-MS) technology for determination of stilbene series hormone,including hexestrol,dienoestrol and diethylstilbestrol in cosmetics was established.The sample was purified with solid phase extraction and analyzed by HPLC-MS under multiple reactions monitoring(MRM).After comparison of experimental results,the chromatography column was selected as Phenomenex Luna C18.Mobile phase fluid was selected as acetonitrile and water with flow rate of 200 μL·min-1.In the beginning of elution,the water volume fraction was 70% and carried out for 4 min,and then the water volume fraction reduced to 20% and carried out up to 7 min.Detection limits of the method for the three kinds of hormone are identified as all 0.125 ng·g-1,and the quantification limits are identified as all 0.25 ng·g-1.The overall recovery varies from 87.5%~100.3% at two spiking level 1.25 and 12.5 ng·g-1.Relative standard deviation of the method ranges between 2.9% and 4.7%(n=15).