QuEChERS-高效液相色谱-串联质谱法测定鸡蛋中38种药物残留

Determination of 38 kinds of veterinary drugs in eggs by QuEChERS and high performance liquid chromatography tandem mass spectrometry

中文关键词:  鸡蛋  多残留检测  液相色谱-串联质谱法  QuEChERS

英文关键词:eggs  multi-residues  liquid chromatography-tandem mass spectrometry  QuEChERS

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定鸡蛋中38种药物残留的分析方法。方法 样品采用0.1 mol/L乙二胺四乙酸二钠(ethylene-diamine-tetra-acetate, EDTA)和乙腈提取, 经QuEChERS净化后, 通过LC-MS/MS测定, 外标法定量。结果 鸡蛋中38种药物在0.3~100 μg/kg浓度范围内相关系数(r2)在0.99138~0.99989之间, 线性关系良好。方法检出限0.05~1.0 μg/kg, 定量限0.1~3.0 μg/kg, 在3.0、10.0、50.0 μg/kg 3个添加水平的平均回收率72.49%~114.06%, 相对标准偏差(n=6)2.37%~13.85%。结论 本方法操作简便快速、灵敏稳定, 适用于鸡蛋中多种药物残留的高通量快速检测。

英文摘要:

      Objective To establish a method for determination of 38 kinds of veterinary drugs in eggs by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The sample was extracted with 0.1 mol/L EDTA and acetonitrile, and cleaned up by QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction method. Then determination of the analytes was performed by LC-MS/MS in negative and positive ionization mode using an electrospray ionization source adopting the multi-reaction monitoring mode. Quantitative was achieved by an external standard method. Results The correlation coefficient (r2) of 38 kinds of drugs in eggs was 0.99138-0.99989 in the concentration range of 0.3?100 μg/kg, and the linear relationship was good. Methods the detection limit was 0.05?1.0 μg/kg, the quantitative limit was 0.1?3.0 μg/kg. The average recoveries of the 38 veterinary drugs were ranged from 72.49% to 114.06% at 3 spiked levels of 3.0, 10.0 and 50.0 μg/kg, with the relative standard deviations (RSDs) in the range of 2.37%-13.85%. Conclusion The proposed method is simple, fast, sensitive and accurate, which is suitable for fast high-throughput detection of multiple residues in eggs.