LC-MS/MS和UPLC-LTQ/Orbitrap MS测定化妆品中糖皮质激素  

Study on detection of glucocorticoids in cosmetics by LC-MS/MS and UPLCLTQ/Orbitrap MS

作　　者：李红英 刘芸 汪薇 吕稳 李丽霞 王会霞 丁晓萍 Ll Hongying;LIU Yun;WANG Wei;LV Wen;Ll Lixia;WANG Huixia;DING Xiaoping(Hubei Institute for Drug Control,Wuhan 430075;Hubei Provincial Institute for Food Supervision and Test,Wuhan 430075)

机构地区：[1]湖北省药品监督检验研究院,武汉430075 [2]湖北省食品质量安全监督检验研究院,武汉430075

出　　处：《分析试验室》2020年第12期1443-1449,共7页Chinese Journal of Analysis Laboratory

基　　金：湖北省药品监督管理局项目(201801009)资助。

摘　　要：采用液相色谱-串联质谱法(LC-MS/MS)测定了化妆品面膜中糖皮质激素类物质,并对检测出现的疑似结果采用高分辨质谱(UPLC-LTQ/Orbitrap MS)进行确证分析。样品经提取净化处理后,分别以ACQUITY UPLC HSS T3 C18和Agilent PFP120为分析柱,0.1%乙酸水溶液和0.1%乙酸-乙腈为流动相,梯度洗脱分离;LC-MS/MS质谱采用正离子模式,多反应监测模式进行检测;UPLC-LTQ/Orbitrap MS采用全扫描和数据依赖扫描模式进行监测。LC-MS/MS检测结果显示,2批样品分别检出保留时间与阿氯米松双丙酸酯(ACDP)和倍他米松(BM)标准品一致的质谱峰,且丰度比在标准允许误差范围内;通过UPLC-LTQ/Orbitrap MS的精确分子量和二级碎片确证了样品中不含阿氯米松双丙酸酯和倍他米松,为基质中物质干扰导致的LC-MS/MS检测结果假阳性。在化妆品检测中,为避免假阳性,有必要使用高分辨质谱等其它方法对检出结果进行确证。The glucocorticoids in facial mask cosmetics was determined by liquid chromatography-tandem mass spectrometry(LC-MS/MS),and the false positive results were identified by linear ion trap/orbitrap mass spectrometry(UPLC-LTQ/Orbitrap MS).The samples were extracted with the saturated solution of sodium chloride and acetonitrile,and purified by solid phase extraction(SPE)column.The analysis was performed on a HSS T3 C18 and a Agilent PFP120 column using 0.1%acetic acid-water solution and 0.1%acetic acidacetonitrile as the mobile phase for gradient elution.The samples were determined by MS under the positive ion mode with the multiple reaction monitoring mode(MRM).High resolution mass spectrometric analysis was performed using both full MS and secondary data dependence mode.Two peaks were similar to betamethasone(BM)and alclometasonedipropionate(ACDP)detected by LC-MS/MS in the two batches of samples,and their retention time were consistent with the standards and the errors of abundance were within permissible values.However,BM and ACDP were not found by UPLC-LTQ/Orbitrap MS.In order to avoid the false positive results for the determination of glucocorticoids in cosmetics using LC-MS/MS,it is necessary to confirm the results by other methods such as high resolution MS.

关 键 词：化妆品 阿氯米松双丙酸酯 假阳性 LC-MS/MS UPLC-LTQ/Orbitrap MS 

分 类 号：O657.31[理学—分析化学] X832[理学—化学]