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 residues in foods of animal origin by QuEChRES dispersive solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry

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(100 mm×2.1 mm,1.8μm)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(r^(2)≥0.9957)。检出限(limits of detection,LODs)为0.05~0.19μg/kg,定量限(limits of quantification,LOQs)为0.17~0.64μg/kg,回收率为61.5%~112.1%,相对标准偏差(relative standard deviations,RSDs)小于等于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奥美普林、利凡诺、磺胺乙氧基哒嗪的快速筛查、定性与定量分析。

Objective To develop a method for the determination of 3 kinds of new veterinary drug residues(ormetoprim,acrinol,and sulfaethoxypyridazine)in food of animal origin by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The food of animal origin was extracted with 85%acetonitrile and separated on an ACQUITY UPLC HSS T3 column(100 mm×2.1 mm,1.8μm).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 4 kinds of matrices of beef,chicken,shrimp,and fish presented a good linear relationship in the range 0.1–50.0 ng/mL(r^(2)≥0.9957).The limits of detection(LODs)were in the range of 0.05–0.19μg/kg,and the limits of quantification(LOQs)were in the range of 0.17–0.64μg/kg,the recoveries were 61.5%–112.1%,and the relative standard deviations(RSDs)were less than or equal to 16.2%.Conclusion The method is simple,sensitive,and suitable for the rapid screening,qualitative and quantitative analysis of ormetoprim,acrinol,and sulfaethoxypyridazine in animal-derived foods.