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

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

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。

Objective： To establish an ultra performance liquid chromatographytandem 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 （r^2 〉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.