超高效液相色谱-串联质谱法测定化妆品中苯菌灵和多菌灵

目的:建立超高效液相色谱-串联质谱(UPLC-MS/MS)法测定化妆品中微量苯菌灵和多菌灵的方法。方法:试样用甲醇-盐酸水溶液提取后,经正己烷萃取除去脂溶性杂质,以混合机理的阳离子固相萃取柱净化、富集,最后C18色谱柱分离,采用UPLC-MS/MS电喷雾电离(ESI),正离子,多反应监测(MRM)模式检测,外标法定量。结果:在1 ng/ml～100 ng/ml范围内,线性关系良好,r2优于0.99;添加回收率范围为82.0%～95.6%,相对标准偏差(RSD)小于4.8%,定量下限为1.0μg/kg。结论:该方法适合各类化妆品中苯菌灵和多菌灵的测定。

Determination of benomyl and carbendazim in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry

Objective:To establish an ultra performance liquid chromatography-tandem mass spectrometric method for determination of benomyl and carbendazim in cosmetics.Methods:The samples were extracted with methanol aqueous solution of hydrochloric acid,the fat-soluble impurities were extracted with hexane,and then purified and enriched with MCX solid phase extraction.The sample solution was injected into UPLC-MS/MS.The analysis was carried out in the multiple reaction monitoring(MRM) mode by employing the external standard method.Results:Within 1 ng/ml～100 ng/ml,the method showed good linearity(r2>0.99).The average recoveries were between 82.0%～95.6% with RSD less than 4.8%.The limit of quantitation(LOQ) was 1.0 μg/kg.Conclution:The method could be used as a reliable means for quantitative determination of benomyl and carbendazim in cosmetics.