【摘要】 目的建立水产品中孔雀石绿、结晶紫及其代谢物（隐色孔雀石绿和隐色结晶紫）的超高效液相色谱-串联质谱测定方法。方法样品加入内标物D5-孔雀石绿和D6-隐色孔雀石绿,经乙腈提取、离心、中性氧化铝固相萃取小柱净化,氮气吹至近干,初始流动相定容后,以BEH C₁₈（2.1 mm×100 mm,1.7μm）色谱柱分离,在电喷雾正离子多反应监测（MRM）模式下检测,采用基质加标工作曲线和内标法定量。结果孔雀石绿、结晶紫、隐色孔雀石绿和隐色结晶紫在0.1μg/L²0.0μg/L时线性关系良好,方法检出限和定量限分别为0.02μg/kg和0.06μg/kg;在0.50μg/kg、2.00μg/kg、10.00μg/kg 3个加标水平下,4种待测物的平均回收率为90.0%¹08.0%,测定结果的相对标准偏差均<10%。结论该方法重现性好、灵敏度高、定量准确,适用于水产品中痕量孔雀石绿、结晶紫及其代谢物残留的检测。更多还原

【Abstract】 Objective To developed a method for the determination of malachite green（ MG）,crystal violet（ CV） and their metabolites,leuco malachite green and leuco crystal violet in aquatic product by ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-MS/MS）. Methods The samples were spiked with D5-malachite green and D6-leuco malachite green as internal standards,then extracted with acetonitrile,purified with neutral alumina solid-phase column,blown almost dry under a stream of nitrogen and dissolved in initial mobile phase. The separation was conducted on a BEH C₁₈（ 2. 1 mm ×100 mm,1. 7 μm） column. The detection was operated by electrospry ionization mass spectrometry in the positive mode under MRM mode,matrix spiked standard calibration curve and internal standard method were employed for quantitative analysis.Results Good linearity was found when the concentrations of them were within 0. 1 μg/L-20. 0 μg/L. The limits of detection（ LOD） and that of quantitation（ LOQ） were 0. 02 μg/kg and 0. 06 μg/kg respectively. The average recoveries were within90. 0%-108. 0% at spiked concentrations of 0. 5 μg/kg,2. 0 μg/kg and 10. 0 μg/kg,with relative standard deviation less than 10%. Conclusion The developed method was selective,sensitive and accurate. It is suitable for the determination of trace MG,CV and their metabolite residues in aquatic product.更多还原