液相色谱-四极杆-线性离子阱质谱仪联用法对护肤类化妆品中7种性激素的快速筛查Rapid Screening and Confirmation of 7 Sex Hormones in Cosmetics by High Performance Liquid Chromatography-Q-Trap Mass Spectrometry
许波;苌玲;
XU Bo;CHANG Ling;Guizhou Institute for Food and Drug Control;
摘要(Abstract):
目的:建立液相色谱-四极杆-线性离子阱质谱(LC-Q-Trap)法测定护肤类化妆品中7种性激素含量的方法。方法:样品用含1.0%乙酸的乙腈溶液超声溶解,用C18柱(2.1 mm×100 mm,1.7μm)分离,乙腈和0.1%乙酸为流动相梯度洗脱,用正、负离子模式同时扫描检测样品中7种性激素含量。结果:7种性激素在0.060 06~1.008 9 mg/L范围内呈良好的线性相关性,相关系数均大于0.9991,定量限为2.0~5.0μg/L,平均回收率为88.7%~110.7%,相对标准偏差为2.7%~6.2%。结论:LC-Q-Trap联合检测方法适用于化妆品中性激素的快速筛查和测定。
Objective: To establish a method for determination of sex hormone in cosmetics with high performance liquid chromatography-Q-Trap(LC-Q-Trap) mass spectrometry.Method: Samples were ultrasonic dissolved in 1.0% acetic acid(in acetonitrile) and separated on C18 column(2.1mm × 100mm,1.7μm),and eluted by using acetonitrile,and 0.1% acetic acid as mobile phase;The mass analyzer was performed in positive and negative full scan modes in one injection at the same time.Results: The linear ranges of the 7 sex hormones were 0.060 06 ~ 1.008 9 mg /L with correlation coefficients above 0.999 1.The limits of quantification were 2.0 ~ 5.0 μg / L,and the recoveries were 88.7 ~ 110.7% % with relative standard deviations of 2.7 ~ 6.2%.Conclusion: LC-Q-Trap combined method is suitable for rapid screening and determination of sex hormones in cosmetics.
关键词(KeyWords):
化妆品;性激素;高效液相色谱-四板杆-线性离子阱质谱法;超声处理
cosmetics;sex hormones;high performance liquid chromatography-Q-Trap mass spectrometry;sonication
基金项目(Foundation): 贵阳市科技局科技计划项目(201210379)号
作者(Author):
许波;苌玲;
XU Bo;CHANG Ling;Guizhou Institute for Food and Drug Control;
Email:
DOI: 10.19367/j.cnki.1000-2707.2013.05.009
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文章评论(Comment):
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- 化妆品
- 性激素
- 高效液相色谱-四板杆-线性离子阱质谱法
- 超声处理
cosmetics - sex hormones
- high performance liquid chromatography-Q-Trap mass spectrometry
- sonication