QuEChERS结合高效液相色谱-串联质谱法同时测定黄颡鱼中7种染料类兽药残留

Simultaneous determination of residues of 7 kinds of dye veterinary drugs in Pelteobagrus fulvidraco fish by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  高效液相色谱-串联质谱法  黄颡鱼  染料  兽药

英文关键词:QuEChERS  high performance liquid chromatography-tandem mass spectrometry  Pelteobagrus fulvidraco fish  dye  veterinary drugs

中文摘要:

      目的 建立黄颡鱼中孔雀石绿、隐色孔雀石绿、结晶紫、隐色结晶紫、亚甲基蓝、天青A、天青B残留量检测的QuEChERS-高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)联用方法。方法 样品中加入乙腈于?18 ℃冷冻30 min, 再加入去水剂无水硫酸镁和氯化钠, 漩涡振荡离心后取上清液加入净化萃取试剂, 漩涡离心后氮气吹至近干, 乙腈复溶并注入HPLC-MS/MS测试。结果 在最优的条件下, 7种染料类兽药在0.1~10 ng/mL范围内线性关系良好, 方法平均回收率为78.2%~95.3%, 精密度为3.0%~5.6%。结论 该方法简单、快速、可靠, 线性关系良好, 检出限低, 灵敏度高, 可用于黄颡鱼中7种染料类兽药残留测定。

英文摘要:

      Objective To establish a method for determination of malachite green, leucomalachite green, crystal violet, leucocrystal violet, methylene blue, azure A and azure B in Pelteobagrus fulvidraco fish using QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Acetonitrile was added into the sample and frozen at ?18 ℃ for 30 min. Then the dehydrating agent anhydrous magnesium sulfate and sodium chloride were added. Supernatant was added to the purification and extraction reagent after vortex oscillation centrifugation. After vortex centrifugation, nitrogen was blown to nearly dry, and acetonitrile was redissolved and injected into HPLC-MS/MS for testing. Results Under optimized conditions, 7 kinds of dye veterinary drugs had good linear relationships in the range of 0.1?10 ng/mL. The recoveries were 78.2%?95.3%, with the relative standard deviations of 3.0%?5.6%. Conclusion This method is simple, rapid, reliable, and with low limit of detection and high sensitivity, which can provide a reference for the determination of residues of 7 kinds of dye veterinary drugs in fish.