超高效液相色谱—飞行时间质谱仪筛查动物源性食品中165种兽药残留

Screening of 165 Animal Drug Residues in Food of Animal Origin by Ultra Chromatography-time of Flight Mass Spectrometry

利用超高效液相色谱—飞行时间质谱仪筛查动物源性食品中165种兽药残留。采用含0.2%甲酸的乙腈∶水(8∶2)作为提取剂,Oasis PRIME HLB通过式净化,以甲醇(含0.1%甲酸)和2.0 mmol甲酸铵溶液(含0.1%甲酸)为流动相梯度洗脱,采用Waters Acquity HSS T3 UPLC色谱柱(100 mm×2.1 mm,1.7μm)分离,电喷雾离子源MSE正离子模式下进行扫描,根据化合物的保留时间、母离子和子离子碎片信息鉴定165种化合物。在猪肉、鱼肉、鸡肉、鸡蛋4种基质165种化合物的平均回收率在53.15%~132.35%。该方法前处理方法简单,能在短时间内实现大批量样品的处理和筛查定性,筛查结果准确可靠,可应用于实际样品的检测。

A rapid screening method for 165 veterinary drug residues in food of animal origin was developed using UPLC-Q-TOFMS.Acetonitrile∶water(8∶2)containing 0.2%formic acid was used as the extractant,and Oasis PRIME HLB was cleaned up by type.The separation was performed on a Waters Acquity HSS T3 UPLC column(100 mm×2.1 mm,1.7μm)with a gradient elution of methanol(containing 0.1%formic acid)and 2.0 mmol/L ammonium formate solution(containing 0.1%formic acid)as the mobile phases,and the compounds were scanned by an electrospray ionization source MSE in the positive mode according to the retention time,parent ion and daughter ion fragmentation information to identify 165 compounds.The average recoveries of 165 compounds in 4 substrates of pork,fish,chicken and egg ranged from 53.15%to 132.35%.The method is simple in pre-treatment,can realize the processing and screening characterization of large volume samples in a short time,and the screening results are accurate and reliable,which can be applied to the detection of real samples.