QuECHERS-HPLC-MS/MS测定祛痘化妆品中7种硝基咪唑类抗菌药物

目的建立测定祛痘化妆品中硝基咪唑类抗菌药物甲硝唑、地美硝唑、洛硝哒唑、异并硝唑及其代谢物羟基甲硝唑、羟基二甲硝咪唑和羟基异丙硝唑的方法。方法试样用0.1%甲酸乙腈溶液提取,通过QuEChERS净化后过滤膜上机检测,以ZORBAX SB-C18色谱柱分离,0.1%甲酸乙腈-0.1%甲酸水溶液作为流动相梯度洗脱,电喷雾正离子模式(ESI+),多重反应监测(MRM)扫描,外标法定量。结果 7种目标分析物在5.0~500.0ng·mL^-1内与峰面积均呈良好线性关系,相关系数均>0.995,在3个不同浓度添加水平下,平均加样回收率为87.9%~114.9%,相对标准偏差RSD(n=6)为0.4%~4.5%。方法的定量限为5~40μg·kg^-1,最低检测限为1.4~12.0μg·kg^-1。结论该方法具有净化效果好、操作简单、准确快速的特点,适用于祛痘化妆品中硝基咪唑类抗菌药物及其代谢物的检测。

Determination of Seven Nitroimidazole Antibiotics in Acne Dispelling Cosmetics by QuECHERS-HPLC-MS/MS

OBJECTIVE To establish a determination method for metronidazole,dimetridazole,ronidazole,ipronidazole and their metabolites 1-(2-hydroxyethyl)-2-hydroxy-methyl-5-nitroimidazol,2-hydroxymethyl^-1-methyl-5-nitroimidazole and hydroxy-ipronidazole in acne dispelling cosmetics.METHODS The sample was extracted with 0.1% formic acid-acetonitrile,and then purified by QuECHERS method.The separation and analysis was performed on a ZORBAX SB-C18 column.The mobile phase consisted of 0.1% formic acid acetonitrile-0.1% formic acid aqueous solution by gradient elution,electrospray ionization(ESI) source was applied and operated in the positive mode.Multiple reaction monitoring(MRM) mode was used to monitor ions.External standard method was used to quantitative calculation.RESULTS Seven target analytes showed good linear relationship in the range of 5.0-500.0 ng·mL^-1.The linear correlation coefficients of the method were > 0.995.At three levels,the average recoveries ranged from 87.9% to 114.9%,with the RSD(n=6) from 0.4% to 4.5%.The limits of quantification of the method were among 5-40 μg·kg^-1,and the limits of detection were among 1.4^-12.0 μg·kg^-1.CONCLUSION This method has good purification effect,it is simple and rapid,which can be applied to the detection of nitroimidazoles antibiotics and their metabolites in acne dispelling cosmetics.