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

作　　者：赖俊敏 赵思雯 李思源[1] 严小红[1] 丁怡[1] LAI Junmin;ZHAO Siwen;LI Siyuan;YAN Xiaohong;DING Yi(Guangzhou Institute for Drug Control,Guangzhou 510160,Guangdong,China)

机构地区：[1]广州市药品检验所,广东广州510160

出　　处：《香料香精化妆品》2024年第6期113-117,共5页Flavour Fragrance Cosmetics

基　　金：广州市市场监督管理局科技项目(编号2023kj30)。

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×0.25μm)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0.5~5μg/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0.05~0.1μg/mL和0.15~0.3μg/mL。在0.5、0.7、1.5μg/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。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.Theα-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×0.25μm),detected by GC-MS/MS in multiple reaction monitoring(MRM)mode,and quantified by external standard method.Results showed that the 7α-hydroxy acids exhibited good linearity within the concentration range of 0.5-5μg/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 0.05-0.1μg/mL and 0.15-0.3μg/mL,respectively.At spiked levels of 0.5,0.7,1.5μg/mL,the recoveries of the 7α-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 ofα-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 

分 类 号：TQ658[化学工程—精细化工] O657.63[理学—分析化学]