超高效液相色谱-串联质谱法同时测定化妆品中8种双酚类及烷基酚类内分泌干扰物  

Simultaneous Determination of Eight Bisphenols and Alkylphenols Endocrine Disruptors in Cosmetics by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：袁晓倩 韩晶[1] 简龙海[1] 陈静[1] 毛北萍[1] 郑荣[1] YUAN Xiao-qian;HAN Jing;JIAN Long-hai;CHEN Jing;MAO Bei-ping;ZHENG Rong(Key Laboratory for Monitoring and Evaluation of Cosmetics,National Medical Products Administration,Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所,国家药品监督管理局化妆品监测评价重点实验室,上海201203

出　　处：《分析测试学报》2020年第7期906-911,共6页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(21874098,81741095,61775157);山西省重点研发计划(国际科技合作)项目(201903D421053);山西省高等学校科技成果转化培育项目;山西省重点研发计划(高新领域)项目(201903D121158)。

摘　　要：建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定化妆品中8种双酚类及烷基酚类化合物含量的分析方法。粉类、水剂、膏霜乳液类、凝胶类化妆品采用乙腈-1%氨水(4∶1,体积比)混合溶液超声提取,经BEH Phenyl色谱柱(2.1 mm×100 mm,2.5μm)分离,用流动相甲醇和0.1%氨水溶液梯度洗脱,在负离子模式下,采用多反应监测(MRM)扫描方式测定。在优化条件下,8种双酚类及烷基酚类化合物在一定质量浓度范围内具有良好的线性关系,线性系数(r)均大于0.997,方法检出限(LOD)为0.00125~0.025 mg/kg,定量下限为0.005~0.05 mg/kg。回收率为75.1%~107%,相对标准偏差(RSD,n=6)为0.1%~1.6%。该方法灵敏度高、通用性强、重复性好,能够有效分离多种同分异构体,适用于同时测定化妆品中的8种双酚类和烷基酚类内分泌干扰物。An ultra-performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS)method was established for the determination of eight bisphenols and alkylphenols in cosmetics.Powders,waters,creams and gel cosmetics were extracted by ultrasonic extraction with acetonitrile-1%ammonium hydroxide solution(4∶1,by volume),then separated on a BEH Phenyl column(2.1 mm×100 mm,2.5μm)by gradient elution with methanol and 0.1%ammonium hydroxide solution as mobile phases,and finally determined in multiple reaction monitoring(MRM)mode.Results showed that the calibration curves for eight bisphenols and alkylphenols exhibited good linear relationships in the certain concentration ranges,with correlation coefficients more than 0.997.The limits of detection(LOD)for eight bisphenols and alkylphenols were in the range of 0.00125-0.025 mg/kg,and the limits of quantitation(LOQ)were 0.005-0.05 mg/kg.The average recoveries were in the range of 75.1%-107%,with relative standard deviations(RSD,n=6)of 0.1%-1.6%.This method is sensitive,versatile and reproducible,and is suitable for the separation of isomers and the simultaneous determination of eight bisphenols and alkylphenols endocrine disruptors in cosmetics.

关 键 词：超高效液相色谱-串联质谱法(UPLC-MS/MS) 化妆品 双酚类 烷基酚类 内分泌干扰物 

分 类 号：O657.63[理学—分析化学] O625.31[理学—化学]