超高效液相色谱-串联质谱法测定防脱发类化妆品中非那雄胺等35种禁用原料

Determination of 35 Prohibited Drugs in Hair Loss Prevention Cosmetics by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

为了评估防脱发类化妆品中是否违禁添加禁用原料,建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定防脱发类化妆品中非那雄胺等35种禁用原料的分析方法。待测样品经饱和氯化钠溶液分散,乙酸乙酯提取,氮吹后以30%乙腈溶液复溶;选用ZORBAX Eclipse Plus C18色谱柱(100 mm×30 mm,1.8μm),乙腈-水流动相体系,在电喷雾(ESI)正负离子模式下以多反应监测(MRM)进行测定。结果显示,在精华液、洗发香波两个基质中,35种组分在各自相应浓度范围内呈良好的线性关系,相关系数(r)均大于0.99。样品在3个浓度加标水平下的回收率为83.2%~118.1%,相对标准偏差(RSD)为0.6%~8.9%。检出限为0.05~6μg/kg,定量限为0.2~20μg/kg。该方法准确、灵敏度高,可用于防脱发类化妆品中35种禁用原料的测定分析,为防脱发类化妆品中违禁添加的监管提供技术参考。

In order to evaluate whether prohibited drugs are prohibited in hair loss prevention cosmetics,an ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the simultaneous determination of 35 prohibited drugs in hair loss prevention cosmetics.After dispersing with saturated sodium chloride and extraction with ethyl acetate,the sample was eluted on a ZORBAX Eclipse Plus C18 column(100 mm×3.0 mm,1.8μm)with a mobile phase consisting of water-acetonitrile.For quantitative analysis,the electrospray ionization source was applied to carry out the positive and negative ions scanning with multiple reaction monitoring(MRM)modes.Results showed that there were good linear relationships for 35 prohibited drugs,with correlation coefficients(r)greater than 0.99.The recoveries ranged from 83.2%to 118.1%at three spiked levels,with the relative standard deviations ranging from 0.6%to 8.9%.The limits of detection range from 0.05 to 6μg/kg,and the limits of quantitation range from 0.2 to 20μg/kg.The method can be used for the determination of 35 prohibited drugs in hair loss prevention cosmetics and provides a technical reference for the supervision and administration of prohibited addition of drugs in hair loss prevention cosmetics.