基于基质固相分散萃取-超高效液相色谱-串联质谱技术同时测定眼影和眉笔中5种防腐剂的含量
Simultaneous Determination of Five Preservatives in Eyeshadow and Eyebrow Pencil Based on Matrix Solid Phase Dispersion Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
黄运龙 1华腾辉 1姚天波 2梁龙 2周宏斌 3袁剑辉 1郑琳3
作者信息
- 1. 宁波中盛产品检测有限公司,浙江宁波 315000
- 2. 宁波爱诗化妆品有限公司,浙江宁波 315000
- 3. 宁波检验检疫科学技术研究院,浙江宁波 315048
- 折叠
摘要
建立基质固相分散萃取-超高效液相色谱-串联质谱法检测眼影和眉笔中苯氧乙醇、脱氢乙酸、山梨酸、甲基氯噻唑琳酮和甲基氯异噻唑啉酮 5 种防腐剂的方法.样品与分散剂佛罗里硅土共研磨后,装入萃取小柱,用甲醇-丙酮洗脱萃取,对样品中防腐剂进行提取.采用超高效液相色谱-串联质谱的多反应监测模式(MRM)对 5 种防腐剂进行定性定量检测.这 5 种防腐剂在 1~200 μg/L均呈良好的线性关系,相关系数(R)均大于 0.995,该方法检出限为0.003~0.008 μg/g,定量限为0.009~0.024 μg/g.该方法具有分离快速、操作简单、灵敏度高、重现性好、线性范围宽等优点,能解决眼影、眉笔等黏性易结块样品溶解不完全导致检测结果偏低的问题.
Abstract
A matrix solid-phase dispersion extraction-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was developed for the determination of five preservatives,namely,phenoxyethanol,dehydroacetic acid,sorbic acid,methylchlorothiazolinone,and methylchloroisothiazolinone,in eyeshadow and eyebrow pencil.The samples were co-milled with the dispersant Florian silica and loaded onto an extraction cartridge,and extracted with methanol-acetone elution to extract the preservatives from the samples.The 5 preservatives were qualitatively and quantitatively detected by ultra performance liquid chromatography-tandem mass spectrometry in multiple reaction monitoring(MRM)mode.The method showed good linearity in the range of 1-200 μg/L with the correlation coefficients(R)greater than 0.995.The limits of detection of the method were 0.003-0.008 μg/g,and the limits of quantification were 0.009-0.024 μg/g.The method has the advantages of rapid separation,simple operation,high sensitivity,good reproducibility,and wide linear range,which can solve the problem of low detection caused by incomplete dissolution of viscous and easily agglomerated samples such as eyeshadow and eyebrow pencil.
关键词
基质固相分散萃取/防腐剂/超高效液相色谱-串联质谱法/眼影/眉笔Key words
matrix solid-phase dispersive extraction/preservative/ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)/eyeshadow/eyebrow pencil引用本文复制引用
基金项目
宁波市公益计划(2023S121)
宁波科技服务项目(2020F023)
出版年
2024