分析化学2025，Vol.53Issue(10)：1623-1630,8.DOI:10.19756/j.issn.0253-3820.251160
在线衍生化反应结合小型便携式质谱现场快速分析化妆品中的4种禁用性激素
Rapid On-site Analysis of Four Prohibited Sex Hormones in Cosmetics Using Online Derivatization Reaction and A Miniature Mass Spectrometer
摘要
Abstract
Due to the poor ionization efficiency and the weak mass spectrometry(MS)intensity of weakly polar substances,direct analysis using the traditional electrospray ionization mass spectrometry(ESI-MS)is a big challenge.In this study,a novel rapid on-site detection method of four prohibited sex hormones in cosmetics was proposed using online derivatization strategy coupled with a miniature mass spectrometer.The target substances in the samples were extracted by a custom-made polyaniline/multi-walled carbon nanotube solid-phase microextraction(SPME)probe.The stirring speed was 200 r/min,the extraction temperature was 40℃,and the extraction time was 2 min.A pulled dual-channel θ borosilicate glass capillary emitter was used as the nano-ESI ion source.The SPME probe was inserted into the channel containing methanol in theθborosilicate glass capillary.When the spray voltage was applied,the four sex hormones were desorbed and formed spray microdroplets,which then collided with the hydroxylamine microdroplets generated from the other channel.The microdroplets of reaction product entered into the miniature mass spectrometer for direct analysis.The limits of detection(LOD)and limits of quantification(LOQ)for the four sex hormones were 10-20 ng/mL and 20-50 ng/mL,respectively.The recoveries were from 84.6%to 107.8%with the relative standard deviations(RSD)from 4.1%to 11.6%.Compared to detection without derivatization,the MS signals of the four target substances were increased by 3 to 15 times.This method was simple,rapid,highly efficient and sensitive,and suitable for on-site rapid analysis of weakly polar sex hormones in cosmetics.关键词
衍生化反应/小型便携式质谱/性激素/化妆品/现场分析Key words
Derivatization reaction/Miniature mass spectrometer/Sex hormone/Cosmetics/On-site analysis引用本文复制引用
佟丽丽,胡艳红,杨任游,吕悦广,尚宇瀚,吕庆,张庆,王强,郭项雨..在线衍生化反应结合小型便携式质谱现场快速分析化妆品中的4种禁用性激素[J].分析化学,2025,53(10):1623-1630,8.基金项目
中央级公益性科研院所基本科研业务费专项资金项目(No.2024JK033)和国家市场监督管理总局专项工业与消费品质量安全保障项目资助. Supported by the Basic Research Fund for Central Public Interest Institutes(No.2024JK033)and Industrial and Consumer Goods Quality Safety Assurance Project of SAMR. （No.2024JK033）
