超高效液相色谱-串联质谱法测定化妆品中5种免疫抑制剂  

Quantitative determination of five immunosuppressants in cosmetics by ultra high-performance liquid chromatography-tandem mass spectrometry

作　　者：吴姣娇 刘玉玲 涂晓琴 殷帅 李启艳 黄海萍 WU Jiaojiao;LIU Yuling;TU Xiaoqin;YIN Shuai;LI Qiyan;HUANG Haiping(Hunan Institute for Drug Control,Hunan Engineering&Technology Research Center for Pharmaceutical Quality Evaluation,Changsha 410001,China;Shandong Institute for Food and Drug Control,Jinan 250101,China)

机构地区：[1]湖南省药品检验检测研究院,湖南省药品质量评价工程技术研究中心,长沙410001 [2]山东省食品药品检验研究院,济南250101

出　　处：《分析试验室》2024年第1期51-56,共6页Chinese Journal of Analysis Laboratory

基　　金：湖南省自然科学基金(2021JJ80039)资助。

摘　　要：建立并验证了超高效液相色谱-串联质谱法(UHPLC-MS)同时测定化妆品中他克莫司、吡美莫司、依维莫司、西罗莫司、环孢菌素A这5种免疫抑制剂的方法。样品采用甲醇超声提取,Atlantis dC18(100 mm×2.1 mm,2μm)色谱柱分离,0.1%乙酸-5 mmol/L乙酸铵水溶液和0.1%乙酸-5 mmol/L乙酸铵甲醇溶液为流动相,多反应监测模式下测定,外标法定量。结果表明,这5种免疫抑制剂在0.5~100 ng/mL浓度范围内线性关系良好,方法检出限均低于10 ng/g,在不同化妆品基质中低、中、高3个浓度水平的加标回收率为93.3%~117.4%,相对标准偏差(RSD)为0.4%~7.5%。日内RSD为2.4%~8.4%,日间RSD为3.9%~26%。该方法弥补了化妆品中非法添加违禁物质检测方法的缺失,为化妆品日常监管提供技术支撑。An ultra high-performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS) method for simultaneous determination of five immunosuppressants in cosmetics,including tacrolimus,pimeclimus,everolimus,sirolimus and cyclosporine A,was established and verified.The samples were ultrasound extracted by methanol and separated by an Atlantis dC18 column(100 mm×2.1 mm,2 μm).The mobile phases were 0.1% acetic acid-5 mmol/L ammonium acetate solution and 0.1% acetic acid-5 mmol/L ammonium acetate methanol solution.The target components were quantified by external standard method under positive ion electrospray ionization and multiple reaction monitoring(MRM) mode.The results showed that the five immunosuppressants had good linear relationships in the concentration ranges of 0.5-100 ng/mL,and the detection limits were all lower than 10 ng/g.The recoveries of the five immunosuppressants at three levels of low,medium and high concentrations in different cosmetic substrates were 93.3%-117.4% and the relative standard deviations(RSDs) were 0.4%-7.5%.The intra-day RSDs were 2.4%-8.4%,and the inter-day RSDs were 3.9%-26%.The method makes up for the lack of detection methods for illegal additives in cosmetics,and provides technical support for the daily supervision of cosmetics.

关 键 词：免疫抑制剂 化妆品 超高效液相色谱-串联质谱 

分 类 号：TQ658.2[化学工程—精细化工]