高效液相色谱-质谱联用法快速筛查化妆品中112种禁用药物

Simultaneous and Rapid Screening of 112 Prohibited Drugs in Cosmetics by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了同时筛查确认化妆品中喹诺酮类、糖皮质激素类、硝基咪唑类、四环素类、大环内酯类、磺胺类、头孢类和性激素8类112种禁用药物的高效液相色谱-质谱联用分析方法。试样采用0. 2%甲酸乙腈作为提取液,通过Qu ECh ERS净化后过滤膜上机检测。以0. 2%甲酸水-0. 2%甲酸乙腈溶液为流动相梯度洗脱,C18色谱柱分离,质谱动态多反应监测(DMRM)模式进行分析。结果表明,112种药物的定量下限为2. 0～10. 0μg/kg;加标回收率为82. 0%～108%;相对标准偏差(RSD)为2. 0%～7. 9%。该方法操作简单、快速、高效,适用于化妆品中上述几类禁用药物的快速筛查和测定。

An analytical method was established for the simultaneous screening and determination of 112 prohibited drugs,including quinolones,glucocorticoids,nitroimidazoles,tetracyclines,macrolides,sulfonamides,cephems and androgens in cosmetics by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The sample was extracted with 0.2%formic acid-acetonitrile,and then purified by QuEChERS method.The extracts were separated on an Agilent ZorbaxEclipsePlus C 18(3.0 mm×150 mm,1.8μm)column with 0.2%formic acid-acetonitrile solution containing 0.2%formic acid as mobile phase by gradient elution,and analyzed by LC-MS/MS under dynamic multiple reaction monitoring(DMRM)mode.Results showed that the limits of quantitation(LOQ,S/N=10)for 112 target compounds in cosmetics were in the range of 2.0-10.0μg/kg.The mean recoveries for 112 prohibited drugs were in the range of 82.0%-108%with their RSDs of 2.0%-7.9%.The method has the advantages of simplicity,rapidness and high efficiency,and could be applied in the screening and confirmation on 112 prohibited drugs in cosmetics in routine analysis.