超高效液相色谱-串联质谱法检测鱼类中孔雀石绿、结晶紫及其代谢物

Detection of malachite green, crystal violet and its metabolites in fish by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  孔雀石绿  隐性孔雀石绿  结晶紫  隐性结晶紫  鱼类

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  malachite green  leuco malachite green  crystal violet  leuco crystal violet  fish

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定鱼类中孔雀石绿、结晶紫及其代谢物的分析方法。方法 本方法依据GB/T 19857-2005, 样品用乙腈提取, 分散固相萃取净化管净化后, 采用色谱柱分离。样品经过离子化后进入质谱仪中, 以水和乙腈为流动相, 电喷雾正离子化模式(electrospray ionization, ESI+)和多反应检测(multiple reaction monitoring, MRM)扫描模式进行测定, 同位素内标法定量。结果 孔雀石绿和结晶紫及其代谢产物在0.2～2.0 ng/mL浓度范围内, 线性关系良好(r＞0.999), 检出限均为0.5 μg/kg。在0.5～2.0 μg/kg水平内, 目标物质的平均加标回收率在99.71%～112.86%之间, 相对标准偏差均不超过13%。对72份鱼类样品进行检测, 隐性孔雀石绿的检出率为1.38%, 其余均未检出。结论 该方法定量准确、分析时间短, 适用于鱼肉中孔雀石绿和结晶紫及其代谢物残留量的定量检测。

英文摘要:

      Objective To establish a method for the determination of malachite green, crystal violet and its metabolites in fish by ultra performance liquid chromatography-tandem mass spectrometry. Methods Based on GB/T 19857-2005, the samples were extracted with acetonitrile and purified by d-SPE purification tube. The samples were separated by chromatographic column, and then entered into the mass spectrometer after ionized. Water and acetonitrile were used as the mobile phase, electrospray ionization (ESI+) and multiple reaction monitoring (MRM) scanning mode were used to determine the samples, and the internal standard method was used for quantitative analysis. Results Malachite green, crystal violet and their metabolites showed a good linear relationship (r>0.999) in the concentration range of 0.2?2.0 ng/mL, with detection limits of 0.5 μg/kg. Within the range of 0.5?2.0 μg/kg, the average recoveries of target substances were between 99.71% and 112.86%, and the relative standard deviations were not more than 13%. 72 fish samples were detected, the detection rate of leucomalachite green was 1.38%, the others were not detected. Conclusion The method is accurate and time-consuming. It is suitable for the quantitative determination of malachite green, crystal violet and their metabolites residues in fish.