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作 者:薛霞[1,2,3] 宿书芳[1,2,3] 王骏[1,2,3] 张卉[1,2,3] 祝建华[1,2,3]
机构地区:[1]山东省产品质量监督检验研究院 [2]国家加工食品质量监督检验中心(山东) [3]山东省材料化学安全检测技术重点实验室,济南250103
出 处:《中国卫生检验杂志》2012年第8期1796-1799,共4页Chinese Journal of Health Laboratory Technology
摘 要: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.
关 键 词:超高效液相色谱-串联质谱 苯菌灵 多菌灵 化妆品 多反应监测
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