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超高效液相色谱法测定护手霜中5种不同的雌激素
引用本文:林雪霞,刘艳,张经华,林金明.超高效液相色谱法测定护手霜中5种不同的雌激素[J].中国科学B辑,2009,39(8):832-837.
作者姓名:林雪霞  刘艳  张经华  林金明
作者单位:① 清华大学化学系, 北京100084; ② 北京市理化分析测试中心, 北京100089
基金项目:本工作得到教育部高等学校博士点基金(批准号:20070003026)资助,特此致谢.
摘    要:建立了超声波萃取.超高效液相色谱快速测定护手霜中5种雌激素(雌酮,雌二醇,苯甲酸雌二醇,美雌醇,炔雌醇环戊醚)的分析方法,研究了萃取溶剂、萃取时间对萃取效率的影响,确立了流动相流速及色谱柱柱温等检测条件.化妆品以乙腈和水(20:80,V:V)为提取溶剂进行超声波萃取后用C18色谱柱分离,乙腈和水溶液为流动相,梯度洗脱,10min内完成5种雌激素的分离与检测.方法的检出限为0.016—0.031μg/mL,相对标准偏差均小于5.0%m=3),5种雌激素的工作曲线的相关系数均高于0.992.化妆品的加标回收率在85%~95%之间.方法简单快速、灵敏度高、分离效果好,满足化妆品中雌激素分析的需要.

关 键 词:超声萃取  雌激素  护手霜  超高效液相色谱
收稿时间:2009-05-19
修稿时间:2009-06-26

Simultaneous determination of five estrogens in hand cream by ultra high-performance liquid chromatography
LIN XueXia,LIU Yan,ZHANG JingHua & LIN JinMing.Simultaneous determination of five estrogens in hand cream by ultra high-performance liquid chromatography[J].Science in China(Series B),2009,39(8):832-837.
Authors:LIN XueXia  LIU Yan  ZHANG JingHua & LIN JinMing
Institution:1. The Key Laboratory of Bioorganic Phosphorus Chemistry & Chemical Biology, Department of Chemistry, Tsinghua University, Beijing 100084, China; 2. Beijing Center for Physical and Chemical Analysis, Beijing 100089, China)
Abstract:A simple, sensitive and high through put ultra high-performance liquid chromatography (LCU) method has been developed for the simultaneous determination of five estrogens in hand cream involving novel ultra- sonic-extraction. Six hormones were determined including estrone, 1713-estradiol, 17a-ethynglestradiol-3- cyclopenty ether and 1713-estradiol benzoate. Parameters such as extraction solution and, extracting time had been optimized. The results showed that these parameters affected the stability and validity of the method. Under the optimized con- ditions, a method with good reproducibility (0.44%-5.00%) and the recovery (85%-95%) were developed for target compounds in the cosmetic. The detection limit of the method was ranged from 0.016 μg/mL to 0.031μg/mL. It can be demonstrated that this method was sensitive enough for the detection of these hormones in cosmetic real samples. The calibration curves were linear with correlation coefficient ranged from 0.992 to 0.999.
Keywords:ultrasonic-extraction  estrogens  hand cream  ultra high-performance liquid chromatography
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