香料香精化妆品2024,Issue(6) :113-117.DOI:10.20099/j.issn.1000-4475.2023.0329

BSTFA衍生化-气相色谱-串联质谱法测定化妆品中7种α-羟基酸的含量

Determination of Seven α-Hydroxy Acids in Cosmetics by Gas Chromatography-Tandem Mass Spectrometry after BSTFA Derivatization

赖俊敏 赵思雯 李思源 严小红 丁怡
香料香精化妆品2024,Issue(6) :113-117.DOI:10.20099/j.issn.1000-4475.2023.0329

BSTFA衍生化-气相色谱-串联质谱法测定化妆品中7种α-羟基酸的含量

Determination of Seven α-Hydroxy Acids in Cosmetics by Gas Chromatography-Tandem Mass Spectrometry after BSTFA Derivatization

赖俊敏 1赵思雯 1李思源 1严小红 1丁怡1
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作者信息

  • 1. 广州市药品检验所,广东 广州 510160
  • 折叠

摘要

建立了化妆品中 7 种α-羟基酸的N,O-双-(三甲基硅烷基)三氟乙酰胺(BSTFA)硅烷衍生-气相色谱-串联质谱测定方法.用N,N-二甲基甲酰胺(DMF)提取化妆品中α-羟基酸,经BSTFA硅烷化衍生后,使用 HP-5MS色谱柱(30 m×0.25 mm×0.25 μm)分离,气相色谱-串联质谱仪多反应监测(MRM)模式检测,外标法定量.结果表明,7 种α-羟基酸在 0.5~5 μg/mL线性良好,相关系数均大于 0.994.检测限(LOD)和定量限(LOQ)分别为 0.05~0.1 μg/mL和 0.15~0.3 μg/mL.在 0.5、0.7、1.5 μg/mL加标水平下,水类、乳液类 2 种不同化妆品基质中7种α-羟基酸的平均回收率在81.4%~126.2%,相对标准偏差(RSD)小于15%(n=6).方法基质效应小,准确度高,可用于化妆品中α-羟基酸的测定.

Abstract

A gas chromatography-tandem mass spectrometry(GC-MS/MS)method with N,O-bis-(trimethylsilyl)trifluoroacetamide(BSTFA)silylation derivatization for the determination of 7 α-hydroxy acids in cosmetics was established.The α-hydroxy acids in cosmetics were extracted with N,N-dimethylformamide(DMF),derivatised by BSTFA silylation,separated using HP-5MS column(30 m×0.25 mm×0.25 μm),detected by GC-MS/MS in multiple reaction monitoring(MRM)mode,and quantified by external standard method.Results showed that the 7 α-hydroxy acids exhibited good linearity within the concentration range of 0.5-5 μg/mL,with all correlation coefficients greater than 0.994.The limits of detection(LOD)and quantification(LOQ)were found to be in the ranges of 0.05-0.1 μg/mL and 0.15-0.3 μg/mL,respectively.At spiked levels of 0.5,0.7,1.5 μg/mL,the recoveries of the 7 α-hydroxy acids in 2 different cosmetic matrices,namely aqueous and emulsion-based,ranged from 81.4%to 126.2%.The relative standard deviations(RSDs)were less than 15%(n=6).This method exhibits low matrix effect,high accuracy,and can be used for the determination of α-hydroxy acids in cosmetics.

关键词

BSTFA衍生化法/气相色谱-串联质谱法/α-羟基酸/化妆品

Key words

BSTFA derivatization/gas chromatography-tandem mass spectrometry(GC-MS/MS)/α-hydroxy acids/cosmetics

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出版年

2024
香料香精化妆品
上海香料研究所

香料香精化妆品

CSTPCD
影响因子:0.341
ISSN:1000-4475
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