超高效液相色谱-串联质谱法同时测定化妆品中21种性激素含量  

Simultaneous determination of 21 sexual hormones in cosmetics by ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：林志惠[1] 赵彦[1] 幸苑娜[1] 陈茜[1] 冯岸红[1] 叶淋泉[1] 陈泽勇[1] 

机构地区：[1]深圳市计量质量检测研究院,深圳518109

出　　处：《分析试验室》2017年第4期441-447,共7页Chinese Journal of Analysis Laboratory

基　　金：国家质量监督检验检疫总局科技计划项目(2015QK173)资助

摘　　要：建立了超高效液相色谱-串联质谱法(UHPLC-MS-MS)同时测定化妆品中21种性激素含量的分析方法。水状、乳状、油状的化妆品采用甲醇/乙腈(1∶1,V/V)漩涡提取,利用HLB固相萃取柱净化萃取,选取4 m L乙腈为洗脱液收集样品液后,经C18色谱柱分离,以甲醇-乙腈及0.5 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,采用动态多反应监测(d MRM)扫描方式进行测定。21种性激素成分在25~800 ng/m L范围内呈良好的线性关系,其相关系数(r2)均大于0.999,方法定量限(LOQs)为0.05~0.61 mg/kg。此外,高、低两个浓度加标水平的实验结果表明,方法平均回收率为74%!110%,相对标准偏差(RSD)为1.2%~10%(n=3)。In this paper, a method of ultra high performance liquid chromatography - tandem mass spectrometry （UHPLC-MS-MS） was developed for simultaneous determination of 21 sexual hormones in cosmetics. Various cosmetic samples （lotion, cream and cleansing oil ） were vortex extracted with methanol and acetonitrile （ 1：1, V/V）, purified with HLB solid phrase extraction （SPE） cartridges and collected with 4 mL aeetonitrile. The extracts were separated by C1s column using a gradient elution of methanol-acetonitrile and 0. 5 mmol/L ammonium acetate as mobile phase. The analysis of the target compounds was performed under dynamics multiple reaction monitoring （dMRM）. The method showed a good linearity in the range of 25 - 800 ng/mL with correlation coefficients （r2 ） more than 0. 999, and the limits of detection quantization （LOQs） for 21 target analytes ranging from 0. 05 mg/kg to 0. 61 mg/ kg. Finally, the average recoveries at two spiked concentration levels were found in the range of 74% - 110%, and relative standard deviations （RSDs） ranged from 1.2% -10% （n = 3 ）. The results indicate that the newly established UHPLC-MS-MS method was reliable and sensitive, and thus could be effectively applied to determine 21 sexual hormones in cosmetics.

关 键 词：超高效液相色谱-串联质谱法(UHPLC-MS-MS) 性激素 化妆品 固相萃取(SPE) 

分 类 号：TQ65[化学工程—精细化工]