QuEChRES分散固相萃取-高效液相色谱-串联质谱法测定动物源性食品中3种新型兽药残留

Determination of 3 kinds of novel veterinary drug residues in foods of animal origin by QuEChRES dispersive solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  动物源性食品  多基质  新型兽药残留

英文关键词:High performance liquid chromatography-tandem mass spectrometry  Foods of animal origin  Multi-matrix  Novel veterinary residues

中文摘要:

      目的 建立一种高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定动物源性食品中奥美普林、利凡诺和磺胺乙氧基哒嗪3种新型兽药残留的检测方法。方法 动物源性食品经85%乙腈提取，ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm, 1.8 μm)分离。正离子电喷雾电离(electrospray ionization，ESI)和多离子检测模式(multiple reaction monitoring，MRM)进行检测。以乙腈-5 mmol/L乙酸铵+0.1%甲酸为流动相梯度洗脱，基质匹配外标法定量。结果 经优化，牛肉、鸡肉、虾、鱼肉4种基质中目标兽药残留在0.1~50.0 ng/mL范围内线性关系良好(r2≥0.9957)。检出限(limits of detection, LODs)为0.05~0.19 μg/kg，定量限(limits of quantification, LOQs)为0.17~0.64 μg/kg，回收率为61.5%~112.1%，相对标准偏差(relative standard deviations, RSDs)小于16.2%。结论 该方法操作简单、灵敏度高，适用于动物源性食品中利凡诺、磺胺乙氧基哒嗪、奥美普林的快速筛查、定性与定量分析。

英文摘要:

      Objective To develop a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of 3 new veterinary drug residues(ormetoprim, acrinol, and sulfaethoxypyridazine) in food of animal origin. Methods The food of animal origin was extracted with 85% acetonitrile and separated on an ACQUITY UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm). The detection was conducted using positive ion electrospray ionization (ESI) and multiple reaction monitoring (MRM) mode. The mobile phase gradient elution consisted of acetonitrile and 5 mmol/L ammonium acetate with 0.1% formic acid, and the matrix-matched external standard method was employed for quantification. Results The optimized results showed that the target veterinary residues in the four matrices of beef, chicken, shrimp, and fish presented a good linear relationship in the range 0.1-50.0 ng/mL (r2≥0.9957). The limits of detection (LODs) were in the range of 0.05-0.19 μg/kg, and the limits of quantification (LOQs) were in the range of 0.17-0.64 μg/kg, the recoveries were 61.5-112.1%, and the relative standard deviations (RSDs) were less than 16.2%. Conclusion The method is simple, sensitive, and suitable for the rapid screening, qualitative and quantitative analysis of acrinol, sulfaethoxypyridazine, and ormetoprim in animal-derived foods.