【摘要】 采用液相色谱-串联质谱法(LC-MS/MS)测定了水产品中结晶紫以及它的隐色代谢物残留。匀质后的水产品样品用乙腈和乙酸铵缓冲液提取,合并提取液,用二氯甲烷反提取,经中性氧化铝柱和PRS柱固相萃取净化,且不使用氧化铅柱在线氧化,色谱分离后直接进入串联质谱检测器。采用电喷雾正离子,多反应监测(MRM)模式检测。方法的检出限可达0.5 ng/g,线性方程的相关系数r大于0.99,添加样品平均回收率为77.6%~93.8%,相对标准偏差均小于8.2%。更多还原

【Abstract】 A liquid chromatography tandem mass spectrometry（LC-MS/MS） method was described for determination of residues of crystal violet（CV） and its metabolite leucocrystal violet（LCV） in aquatic products.The targeted analytes were extracted from homogenized samples with a mixture of acetonitrile and ammonium acetate buffer,partitioned against methylene chloride,and purified on tandem neutral alumina and PRS SPE cartridges.Chromatographic Separation was achieved by using ZORBAX SB-C₁₈ column with an isocratic mobilc phase consisting of ammonium acetate（0.05 mM） and acetonitrile（10/90,V/V） without post-column oxidation with PbO₂.Identification and quantification were performed using multiple reaction monitoring（MRM） with one precursor ion and two productions for each analyte and electrospray ionization in positive mode.The detection limit was 0.5 ng/g.and correlation coefficient of linear regression equations were above 0.99.Recoveries were in the range of 77.6%⁹3.8% and the RSD were less than 8.2%.更多还原