固相萃取/超高效液相色谱-串联质谱法测定化妆品中5种防晒剂  

Determination of five sunscreens in cosmetics by solid phase extraction/ultra-high performance liquidchromatography-tandem mas spectrometry

作　　者：李欣[1] 李帮锐[1] 冯家力[1] 曾栋[1] 陈东洋[1] LI Xin;LI Bangrui;FENG Jiali;ZENG Dong;CHEN Dongyang(Physical&Chemical Laboratory Department,Hunan Center for Disease Control and Prevention,Changsha Hunan,410005,China)

机构地区：[1]湖南省疾病预防控制中心理化检验科,湖南长沙410005

出　　处：《职业与健康》2023年第17期2345-2349,共5页Occupation and Health

摘　　要：目的开发固相萃取/超高效液相色谱-串联质谱技术,用于测定化妆品中5种防晒剂的含量。方法样品通过固相萃取净化、富集处理,采用超高效液相色谱对其中5种防晒剂进行分离,质谱多反应监测(multi-reaction monitoring,MRM)模式测定。结果对苯二亚甲基二樟脑磺酸、苯亚二苯并咪唑磺酸酯二钠和苯二酮-4在1μg/L~10 mg/L范围内,亚苄基樟脑磺酸、苯基苯并咪唑磺酸在0.5μg/L~5 mg/L范围内,峰面积与浓度线性关系良好,回归方程相关系数(r)≥0.9993。5种防晒剂加入低、中、高3个浓度水平进行加标回收率实验,5种防晒剂回收率在91.7%~102.5%之间,相对标准偏差在2.6%~4.9%之间。对苯二亚甲基二樟脑磺酸、苯亚二苯并咪唑磺酸酯二钠和苯二酮-4的方法检出限为0.001 mg/kg,定量限为0.002mg/kg。亚苄基樟脑磺酸、苯基苯并咪唑磺酸的方法检出限为0.0005 mg/kg,定量限为0.001 mg/kg。对市售不同类型共6批次的化妆品样本进行了检测,测定结果均未超出国家限量值。结论本方法用含2%甲酸的90%丙酮溶液作为提取剂,采用混合型弱阴离子交换柱对化妆品中5种防晒剂净化、富集,有效降低了基质干扰,配合液质联用技术,提高了待测化合物测定的准确度。样品实测表明,方法简便快速、灵敏度高、线性范围宽、抗干扰能力强,而且可实现样本前处理自动化。Objective To explore solid phase extraction/ultra-high performance liquid chromatography-tandem mass spectrometry technique for the content determination of 5 sunscreens.Methods The samples were purified and enriched by solid phase extraction,and the 5 sunscreens in cosmetics were separated by ultra-high performance liquid chromatography,and measured by mass spectrometry with multi-reaction monitoring(MRM)mode.Results The p-benzenedimethylene-dicamphorsulfonic acid,benzimidazole sulfonate disodium and benzophenone-4 were in the range of 1μg/L to 10 mg/L,and benzylidene-camphorsulfonic acid,phenylbenzimidazole sulfonic acid were in the range of 0.5μg/L to 5 mg/L,there was a good linear relationship between peak area and concentration,and the correlation coefficient of regression equation(r)≥0.9993.5 sunscreens were tested at low,medium and high concentration levels to carry out the recovery experiment.The recovery rate of 5 sunscreens was between 91.7%and 102.5%,and the relative standard deviation was between 2.6%and 4.9%.The detection limits and quantitative limits of pbenzenedimethylene-dicamphorsulfonic acid,benzimidazole sulfonate disodium and benzophenone-4 were 0.001 and 0.002 mg/kg,respectively.The detection limits of benzylidene-camphorsulfonic acid,phenylbenzimidazole sulfonic acid was 0.0005 mg/kg,and the quantitative limits was 0.001 mg/kg.6 batches of cosmetics samples with different types in the market were determined,and the results did not exceed the national limit.Conclusions In this method,90%acetone solution containing 2%formic acid was used as extractant,and five sunscreens in cosmetics were purified and enriched by mixed weak anion exchange column,which effectively reduced matrix interference and improved the accuracy of determination with solid phase extraction/ultra high performance liquid chromatography-tandem mass spectrometry.The actual measurement of samples showed that the method was simple,rapid,sensitive,and had wide linear range and strong anti-interference ability,and could reali

关 键 词：超高效液相色谱-串联质谱 固相萃取 化妆品 防晒剂 

分 类 号：R115[医药卫生—公共卫生与预防医学]