液相色谱-串联质谱法测定化妆品中22种激素  

LC-MS/MS Determination of 22 Hormones in Cosmetics

作　　者：陈溪 张晓林 刘莹 崔晗 黄大亮 林维宣[2] 

机构地区：[1]大连出入境检验检疫局庄河办事处,庄河116400 [2]辽宁出入境检验检疫局,大连116000

出　　处：《理化检验（化学分册）》2013年第4期468-472,476,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质检总局科研课题(2009IK149-2)

摘　　要：提出了采用液相色谱-串联质谱法测定化妆品中22种激素残留量的方法。样品经乙腈超声提取,分别采用Oasis HLB固相萃取柱(方法一)和凝胶渗透色谱(方法二)两种方法净化。经净化的试液用ZORBAX Eclipse XDB-C18色谱柱(100mm×2.1mm,1.8μm)分离,15种激素用不同比例配成的含0.1%(体积分数)甲酸的水溶液和乙腈组成的流动相梯度洗脱。质谱测定中采用正离子电离方式多反应监测模式;另7种激素用不同比例配成的水和乙腈组成的流动相梯度洗脱,质谱测定中采用负离子电离方式多反应监测模式。方法一的检出限为0.01～0.40mg.kg-1;回收率在61.5%～111%之间;方法二的检出限在0.1～4.0mg.kg-1之间,回收率在60.8%～113%之间。LC-MS/MS was applied to the determination of residual amounts of 22 hormones in cosmetics. The sample was ultrasonically extracted with aeetonitrile, and purified hy Oasis HLB solid-phase extraction column （method 1） and gel permeation chromatography （method 2） separately. The hormones in the purified solution were separated on ZORBAX Eclipse XDB-C18 （ 100 mm × 2. 1 mm, 1.8 μm） column and eluted by gradient elution. Mixtures of acetonitrile and 0. 1%（φ） formic acid solution with different mixing ratio by volume were used as eluants in the elution, and ESI＋ mode was used in MS determination for 15 of the 22 hormones, and mixtures of acetonitrile and H20 with different mixing ratio by volume were used as eluants in the elution and ESI mode was used in MS determination for the remainder 7 hormones. Multi-reaction monitoring mode was adopted in both the above cases. Values of detection limit （3S/N） found for method 1 were in the range of 0. 01--0.40 mg·kg^-1, while for method 2, were in the range of 0. 1-4.0 mg ·kg^-1. Values of recovery found for method 1 were in the range of 61.5%--111%, while for method 2 were in the range of 60.8%--113%.

关 键 词：液相色谱-串联质谱法 凝胶渗透色谱 化妆品 激素 

分 类 号：O657[理学—分析化学]