建立了分散固相萃取?高效液相色谱?串联质谱（ dispersive?SPE?HPLC?MS／MS）同时测定畜禽肉中β?内酰胺类、喹诺酮类、磺胺类、磺胺类增效剂和抗寄生虫类共5类63种兽药残留的新方法。样品经0?1 mol／L Na2 EDTA溶液及含1％（体积分数）乙酸的乙腈溶液涡旋提取，提取液经C18分散固相萃取净化后，用Poroshell EC?C18色谱柱（100 mm×2?1 mm，2?4μm）分离，在电喷雾离子源正离子模式下以动态多反应监测（DMRM）方式采集数据并做定性筛查和定量分析。63种药物在相应的浓度范围内线性关系良好，相关系数均大于0?99；不同畜禽肉（猪肉、牛肉及鸡肉）在3个不同添加水平下的平均回收率为62?2％～112?0％，相对标准偏差（ RSD）为3?1％～16?3％，检出限（LOD， S／N≥3）和定量限（LOQ， S／N≥10）分别为0?1～3?0μg／kg和0?5～10?0μg／kg。该方法简便快速、灵敏可靠，适用于畜禽产品中兽药多残留的同时快速定性筛查和定量分析。
A novel multiresidue analytical method has been developed and validated for the determination of five classes of veterinary drugs including 18 β?lactams, 15 quinolones, 21 sul?fonamides, 3 sulfonamide potentiators and 6 antiparasitics in meat using dispersive solid?phase extraction ( dispersive?SPE ) and high performance liquid chromatography?tandem mass spec?trometry ( HPLC?MS/MS ) . The analytes were extracted with a vortex mixer by 0?1 mol/L Na2 EDTA solution and acetonitrile containing 1% ( v/v) acetic acid, and then the extracts were purified using dispersive?SPE with C18 sorbent. Electrospray ionization mass spectrometry was operated in positive mode using dynamic multiple reaction monitoring ( DMRM) for the qualita?tive and quantitative analysis of the 63 analytes after the separation on a Poroshell EC?C18 col?umn (100 mm×2?1 mm, 2?4μm). The correlation coefficients of linear calibration curves were over 0?99 in the corresponding concentration ranges. The average recoveries of the 63 analytes ranged from 62?2% to 112?0%, and the relative standard deviations ( RSDs) were 3?1%-16?3%in spiked meat ( pork, beef and chicken muscle) at three levels. The limits of detection ( LODs, S/N≥3) and the limits of quantification ( LOQs, S/N≥10) were 0?1-3?0 μg/kg and 0?5-10?0μg/kg, respectively. The method is simple, rapid, sensitive, reliable and suitable for the deter?mination of residues in animal products.
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