液质联用技术测定化妆品中二苯乙烯类激素  

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

作　　者：郑利[1] 金尉[1] 余雯静[1] 赵玉兰[1] 

机构地区：[1]苏州出入境检验检疫局,江苏苏州215104

出　　处：《日用化学工业》2012年第4期306-309,共4页China Surfactant Detergent & Cosmetics

基　　金：江苏检验检疫局资助项目(2011kj12)

摘　　要：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)。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 Cls- 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 rain, 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）.

关 键 词：化妆品 液相色谱-串联质谱 己烷雌酚 双烯雌酚 己烯雌酚 

分 类 号：TQ658[化学工程—精细化工]