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日用化学工业 ›› 2022, Vol. 52 ›› Issue (1): 84-90.doi: 10.3969/j.issn.1001-1803.2022.01.013

• 分析与检测 • 上一篇    下一篇

气相色谱-质谱/质谱法测定美白化妆品中5种酚类物质

肖昭竞,童兰艳(),李根容,代政华,周朝旭,余文琴   

  1. 重庆市计量质量检测研究院,重庆 401123
  • 收稿日期:2021-03-06 修回日期:2021-12-31 出版日期:2022-01-22 发布日期:2022-01-19
  • 通讯作者: 童兰艳
  • 基金资助:
    重庆市质量技术监督局科研计划项目(CQZJKY2018009)

Determination of five phenolics compounds in whitening cosmetics by gas chromatography-tandem mass spectrometry

Xiao Zhaojing,Tong Lanyan(),Li Genrong,Dai Zhenghua,Zhou Zhaoxu,Yu Wenqin   

  1. Chongqing Academy of Metrology and Quality Inspection, Chongqing 401123, China
  • Received:2021-03-06 Revised:2021-12-31 Online:2022-01-22 Published:2022-01-19
  • Contact: Lanyan Tong

摘要:

建立了同时测定化妆品中苯酚、氢醌、间苯二酚、4-丁基间苯二酚和苯乙基间苯二酚5种酚类物质的气相色谱-质谱/质谱(GC-MS/MS)检测方法。样品在0.03 mol/L磷酸二氢钾溶液中超声提取,经HLB固相萃取小柱净化后,过0.22 μm有机滤膜,采用GC-MS/MS分析。选择SH-Rtx-1701(30 m×0.25 mm×0.25 μm)色谱柱分离,采用EI离子源电离、MRM采集模式,外标法定量。结果表明,5种酚类物质在10 min内完成色谱分离,检出限和定量限分别为1.5~3.0 μg/L和5.0~10.0 μg/L,5种酚类物质在5~200 μg/L范围线性良好,相关系数均大于0.9994,以阴性样品为基质,在不同添加水平下,5种酚类物质的平均回收率为73.5%~111.8%,相对标准偏差(RSD,n=6)在1.0%~11.1%之间。本方法分析时间短,灵敏度好,准确性高、操作方便、净化效果好,可同时测定化妆品中5种酚类物质。

关键词: 气相色谱-质谱/质谱, 固相萃取, 化妆品, 酚类物质

Abstract:

A method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the analysis of 5 phenolics compounds (phenol, hydroquineone, resorcinol, 4-butylresorciol, phenylethyl resorciol) in cosmetics. The phenolics compounds were extracted from cosmetics by supersonic extraction with 0.03 mol/L potassium dihydrogen phosphate solution, purified by HLB solid phase extraction column, and analyzed via GC-MS/MS after filtration with organic filtration membrane (0.22 μm). Separation was performed on a SH-Rtx-1701MS chromatographic column (30 m×0.25 mm×0.25 μm) by GC-MS/MS with an electrospray ionization (EI) source in the MRM mode. The external standard method was used for quantitative determination. The 5 phenolics compounds can be analyzed within 10 min under the optimum conditions, and it exhibits a good linearity with the standard correlation coefficients (R2) of not less than 0.999 in their respective concentration ranges of 5-200 μg/L. The limited of determination (LODs) are 1.5-3.0 μg/L and the limits of quantitation (LOQs) are 5.0-10.0 μg/L, respectively. The recoveries at three standards are 73.5%-111.8%, and the relative standard deviations (RSDs) are between 1.0% and 11.1% (n=6). The proposed method is accurate, reliable, simple and convenient, and is suitable for determination of phenol whitening active components in cosmetics.

Key words: gas chromatography tandem mass spectrometry (GC-MS/MS), solid phase extractions, cosmetics, phenolic compounds (phenols)

中图分类号: 

  • TQ658