QuEChERS-超高效液相色谱-串联质谱法测水产品中多种兽药残留

Determination of Veterinary Drug Residues in Aquatic Products by QuEChERS-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立QuEChERS-超高效液相色谱-串联质谱法同时检测鱼、虾等水产品中磺胺类、喹诺酮类、硝基咪唑类中46种兽药残留的分析方法。样品经1%乙酸乙腈溶液提取,加入PSA和C_(18)进行净化,使用T3色谱柱进行分离,以ESI+电喷雾正离子,MRM扫描模式分析检测,外标法定量。结果表明,46种兽药残留在2~100ng·mL^(-1)具有良好线性关系,相关系数r^(2)>0.99,检出限为0.6~6.0μg·kg^(-1),回收率在60%~119%,相对标准偏差≤7%(n=6)。本方法极大地提高了多种兽药残留检测效率,适用于水产养殖食品安全突发事件应急处置中兽药残留快速分析。

QuEChERS-ultra-high performance liquid chromatography-tandem mass spectrometry was used to establish a method for simultaneous determination of 46 veterinary drugs residues in fish,shrimp and other aquatic products.The sample was extracted by 1%acetonitrile acetate solution,purified by adding PSA and C_(18),separated by T3 column,detected by ESI+electrospray positive ion,MRM scanning mode analysis and detection,external standard method quantification.There was a good linear relationship between the residues of 46 veterinary drugs in the range of 2~100 ng·m L^(-1),the correlation coefficient r^(2)was more than 0.99,the limit of detection was 0.6~6.0μg·kg^(-1),the recoveries were between 60%and 119%,and the relative standard deviation was≤7%(n=6).This method greatly improves the detection efficiency of multi-residue veterinary drugs and is suitable for rapid analysis of multi-residue veterinary drugs in food safety emergencies.