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日用化学工业（中英文）

日用化学工业 ›› 2017, Vol. 47 ›› Issue (8): 476-480.doi: 10.13218/j.cnki.csdc.2017.08.011

• 分析与检测 • 上一篇    

超高效液相色谱-质谱联用法同时测定化妆品中5种禁用性激素

岳磊1, 李晓静2   

  1. 1.郑州市食品药品检验所,河南 郑州 450000;
    2.郑州大学第三附属医院,河南 郑州 450000
  • 收稿日期:2017-04-17 出版日期:2017-08-22 发布日期:2019-03-20
  • 通讯作者: 李晓静,硕士,主管药师,讲师,电话:(0371)66903580,E-mail:lixiaojing2050@163.com。
  • 作者简介:岳 磊(1985-),男,硕士,电话:(0371)68698912,E-mail:15638511@qq.com。
  • 基金资助:
    2015郑州地方高校新世纪教育教学改革及人才培养工程立项(ZZJG-B7027)

Simultaneous determination of five banned sex hormones in cosmetics with UPLC-MS/MS

YUE Lei1, LI Xiao-jing2   

  1. 1.Zhengzhou Institute for Food and Drug Control,Zhengzhou,Henan 450000,China;
    2.Third Affiliated Hospital of Zhengzhou University,Zhengzhou,Henan 450000,China
  • Received:2017-04-17 Online:2017-08-22 Published:2019-03-20

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摘要： 建立了同时测定化妆品中5种禁用性激素的超高效液相色谱-串联质谱法(UPLC-MS/MS)。采用ACQUITY UPLC®BEN C18色谱柱(2.1 mm×50 mm,1.7 μm),流动相为V(甲醇)∶V(0.1%的甲酸水溶液)=60∶40的混合溶液,流速0.4 mL/min,柱温30 ℃,进样量1 μL,扫描方式为多反应监测(MRM)联合相关信息扫描(IDA)与增强离子扫描(EPI)。结果表明,4种雌激素(雌二醇、雌三醇、雌酮和己烯雌酚)及黄体酮的线性范围为1~100 mg/L,方法的线性关系良好,相关系数均大于0.999。样品的平均回收率为79.8%~115.3%,RSD为1.43%~11.36% (n=6)。

关键词: 功效化妆品, 雌激素, 超高效液相色谱-串联质谱法, 多反应监测

Abstract: A method using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established for determination of five banned sex hormones in cosmetics.The chromatography column is selected as ACQUITY UPLC® BEN C18 column (2.1 mm×50 mm,1.7 μm).The mobile phase consists of methanol-0.1% formic acid aqueous solution (60∶40) and the flow rate is 0.4 mL/min.The column temperature is 30 ℃.Sample injection amount is 1 μL.The scanning method is multiple reaction monitoring (MRM) in combination with information dependent acquisition (IDA) and enhanced ion scanning (EPI).Results show that the relation between peak area and mass concentration of the detected four kinds of estrogen,including oestradiol,oestriol,oestrone and stilbestrol as well as progesterone displays good linearity with correlation coefficient higher than 0.999.Detection limit of the method is 1-100 mg/L.The method was carried out at three spiking levels,the average recoveries are in the range of 79.8%-115.3%,with relative standard deviations of 1.43%-11.36% (n=6).

Key words: functional cosmetics, estrogen, ultra-high performance liquid chromatography-tandem mass spectrometry, multiple reaction monitoring

中图分类号: 

  • TQ658