磁性多壁碳纳米管固相萃取/高效液相色谱-串联质谱法测定蜂蜜中多组分兽药残留

Determination of Veterinary Drugs Residues in Honey by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Magnetic Multi-walled Carbon Nanotubes

建立了以磁性多壁碳纳米管为吸附剂的分散固相萃取/高效液相色谱-串联质谱检测方法,对蜂蜜中3大类44种兽药残留进行测定。样品经pH 4.0的Na2EDTA-Mcllvaine缓冲液提取,加入自制磁性多壁碳纳米管吸附目标物。目标物经10%氨水-甲醇洗脱后,液相色谱-串联质谱MRM模式进行定性定量分析。44种药物在1~40 ng/m L浓度范围内线性关系良好,相关系数均大于0.99;在3个不同浓度添加水平下,回收率为78.0%~105.1%,相对标准偏差(RSD)为1.2%~8.9%,检出限为0.2~2.0μg/kg。结果表明,该方法简单方便,易于操作,为蜂蜜中磺胺类、喹诺酮类以及硝基咪唑类兽药残留的测定提供了新途径。

A method using magnetic multi-walled carbon nanotubes（mMWCNTs） as the absorbent followed by ultra-performance liquid chromatography-tandem mass spectrometry was established for the determination of 44 veterinary drugs residues in honey.Analytes were extracted with Na2EDTA-Mcllvaine buffer solution（pH 4.0） before self-made mMWCNTs were added to absorb veterinary drugs.After extraction with mMWCNTs and followed by elution with 10% ammonia-methanol,target analytes were analyzed using multiple reaction monitoring（MRM） mode.The correlation coefficients of linear calibration curves were over 0.99 in the concentration range of 1-40 ng/mL.The recoveries of 44 analytes at three spiked concentrations ranged from 78.0% to 105.1%,with relative standard deviations（RSDs） of 1.2%-8.9%.The limits of detection（LODs,S/N≥3） were 0.2-2.0 μg/kg.With the advantages of simplicity,sensitivity and good precision, this method provides a new way for the determination of multi-veterinary drug residues in honey.