分散固相萃取-高效液相色谱-串联质谱法同时测定畜禽肉中63种兽药残留  

Multiresidue analysis of 63 veterinary drugs in meat by dispersive solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry

作　　者：罗辉泰[1,2] 谢梦婷[1] 黄晓兰[1] 吴惠勤[1] 朱志鑫[1] 黄芳 林晓珊[1] 欧阳钢锋[2] 

机构地区：[1]中国广州分析测试中心,广东省分析测试技术公共实验室,广东广州510070 [2]中山大学化学与化学工程学院,广东广州510275

出　　处：《色谱》2015年第4期354-362,共9页Chinese Journal of Chromatography

基　　金：广州市科技计划项目(11BppZXcc6100034)

摘　　要：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 Na2EDTA 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- unto （ 100 mm×2. 1 mm, 2.4 μm）. 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 ~g/kg and 0.5-10.0 μg/kg, respectively. The method is simple, rapid, sensitive, reliable and suitable for the deter- mination of residues in animal products.

关 键 词：分散固相萃取 高效液相色谱-串联质谱法 β-内酰胺类兽药 喹诺酮类兽药 磺胺类兽药 磺胺类增效剂兽药 抗寄生虫类兽药 畜禽肉 

分 类 号：O658[理学—分析化学]