摘要
该文基于超高效液相色谱-串联质谱法(UHPLC-MS/MS),建立了多种类型化妆品中全氟及多氟化合物(PFASs)的分析方法。水剂、膏霜、乳液、凝胶和粉剂样品经过饱和乙酸铵-氯化钠溶液(含1%甲酸)分散后采用1%甲酸-乙腈溶液提取,油状和蜡基类化妆品经过正己烷分散后采用饱和乙酸铵-乙腈溶液(含0.001%氨水)提取,提取液以Agilent RRHD Eclipse Plus Zorbax C_(18)色谱柱(3.0 mm×100 mm,1.8μm)进行分离,在电喷雾离子源(ESI)下以多反应监测(MRM)模式检测,基质匹配外标法定量。通过考察不同前处理方式对30种PFASs回收率的影响,确定最优前处理方法。在优化条件下,30种PFASs在1~250μg/L范围内呈良好线性关系,相关系数(r^(2))为0.9903~0.9998;方法检出限为0.025~0.125μg/g,定量下限为0.050~0.250μg/g,30种PFASs的平均回收率为70.8%~112%,相对标准偏差(RSD,n=6)为0.50%~12%,24 h内各基质溶液中30种PFASs的峰面积相对标准偏差(RSD)均小于10%。采用该方法对采集的88个化妆品样品进行检测,发现1个阳性样品,检出全氟辛酸(PFOA)和全氟辛基磺酸(PFOS)含量分别为4.7μg/g和1.4μg/g。该方法简便、快速、准确、灵敏,可为化妆品的质量控制和日常监管提供技术支撑。
In this study,a method for the analysis of perfluorinated and polyfluorinated substances(PFASs)in various types of cosmetics was established based on ultra high performance liquid chromatography and tandem mass spectrometry(UHPLC-MS/MS).Lotion,cream,emulsion,gel and powder cosmetics were dispersed by saturated ammonium acetate-sodium chloride solution(containing 1%formic acid)and extracted by 1%formic acid-acetonitrile solution.Oil and wax-based cosmetics were dispersed by n-hexane and extracted by saturated ammonium acetate-acetonitrile solution(containing 0.001%ammonium hydroxide).The extracts were separated on an Agilent RRHD Eclipse Plus Zorbax C_(18) column(3.0 mm×100 mm,1.8μm),analyzed by electrospray ionization source(ESI)under multiple reaction monitoring(MRM)mode and quantified by the matrix-matched calibration.The optimal pretreatment method was confirmed by investigating the recoveries of 30 PFASs under different pretreatment conditions.The method showed a good linear relationship for 30 PFASs in the concentration range of 1-250μg/L,and the correlation coefficients(r^(2))were 0.9903-0.9998.The limit of detection(LOD)and quantitation(LOQ)were 0.025-0.125μg/g and 0.050-0.250μg/g,respectively.The average recoveries of 30 PFASs ranged from 70.8%to 112%,with relative standard deviations(RSDs,n=6)of 0.50%-12%.The RSDs of the peak area of 30 PFASs in each matrix solution within 24 h were less than 10%.This method was applied to the detection of 88 cosmetics samples,and one positive sample was found,whose PFOA and PFOS contents were 4.7μg/g and 1.4μg/g,respectively.The method showed simplicity,rapidity,good accuracy and high sensitivity,which could provide technical support for the quality control and daily supervision of cosmetics.
作者
梁梓洋
张秋炎
周熙
康怀腾
梁韵蕊
轩申鑫
吴惠勤
黄芳
陈桂琴
李杨杰
罗辉泰
LIANG Zi-yang;ZHANG Qiu-yan;ZHOU Xi;KANG Huai-teng;LIANG Yun-rui;XUAN Shen-xin;WU Hui-qin;HUANG Fang;CHEN Gui-qin;LI Yang-jie;LUO Hui-tai(Institute of Analysis,Guangdong Academy of Sciences(China National Analytical Center,Guangzhou),Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology,Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine,Guangzhou 510070,China;Guangdong Institute for Drug Control,National Medical Products Administration Key Laboratory for Safety Risk Assessment of Cosmetics,Guangzhou 510070,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第11期1413-1423,共11页
Journal of Instrumental Analysis
基金
国家药品监督管理局化妆品风险评估重点实验室开放课题(KF2022007)。
关键词
超高效液相色谱-串联质谱(UHPLC-MS/MS)
液液萃取
化妆品
全氟及多氟化合物(PFASs)
全氟化合物
ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)
liquid-liquid extraction(LLE)
cosmetics
perfluorinated and polyfluorinated substances(PFASs)
perfluorinated compound
