UPLC-MS/MS同时检测染发剂中三种二氨基酚类物质  

Determination of 3 diaminophenols in hair dyes by ultra performance liquid chromatography tandem mass spectrometry

作　　者：曹鹏[1,2] 耿金培 许红岩 李晓玉 李金强 梁君妮 沙美兰 

机构地区：[1]烟台出入境检验检疫局,烟台264000 [2]山东农业大学食品科学与工程学院,泰安271018

出　　处：《分析试验室》2011年第10期59-62,共4页Chinese Journal of Analysis Laboratory

基　　金：山东检验检疫局科技计划项目(SK201095)资助

摘　　要：建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测染发剂中三种二氨基酚类物质(2,4-二氨基苯酚盐酸盐、2,4-二氨基苯甲醚盐酸盐、2,3-二氨基苯酚)含量的方法。样品经0.1%甲酸水溶液提取,正己烷净化后,用Waters ACQUITY BEH Shield RP18色谱柱进行分离,流动相为甲醇和5 mmol/L乙酸铵-0.1%甲酸溶液。分离后采用多反应监测模式进行检测,外标法定量。在优化实验条件下,三种化合物的线性范围为10～500μg/L,相关系数均大于0.998。三种二氨基酚类化合物的检出限为3μg/kg,定量下限为10μg/kg,加标平均回收率为80.3%～113.5%,相对标准偏差均不高于8.6%。该方法适用于染发剂中三种二氨基酚类物质的定量及确证分析。An ultra performance liquid chromatography-electrospray ionization triple-quadruple tandem mass spectrometric（UPLC-ESI MS/MS） method has been established for the simultaneous determination of three diaminophenols,including 2,4-diaminophenol dihydrochloride,2,4-diaminoanisole dihydrochloride,and 2,3-Diaminophenol,in hair dyes.The diaminophenols were extracted by water-0.1% formic acid and cleaned up by n-hexane.The separation was carried out by an ACQUITYTM BEH Shield RP18 column using methanol and 5 mmol/L ammonium acetate-0.1% formic acid as the mobile phase.The target compounds were confirmed and quantified by MS-MS under multiple-reaction monitering（MRM） mode with external standard method.Extraction and chromatographic conditions were optimized and the best separation was obtained.Under the optimal conditions,the calibration curves were linear in the range of 10~500 μg/L for the three compounds with correlation coefficients more than 0.998.The limits of detection（LOD） were 3 μg/kg,and the limits of quantitation（LOQ） were 10 μg/kg.The average recoveries of 3 diaminophenols were between 80.3% and 113.5% with the relative standard deviations（RSDs） no more than 8.6%.The proposed method was effective,simple and sensitive,and was suitable for the determination and confirmation of diaminophenols in hair dyes.

关 键 词：超高效液相色谱串联质谱 染发剂 二氨基酚 

分 类 号：O657.63[理学—分析化学]