色谱Issue(4)：354-362,9.DOI:10.3724/SP.J.1123.2014.12005
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
摘要
Abstract
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.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Key words
dispersive solid-phase extraction ( dispersive-SPE)/high performance liquid chro-matography-tandem mass spectrometry ( HPLC-MS/MS)/β-lactam drugs/quinolone drugs/sul-fonamide drugs/sulfonamide potentiator drugs/antiparasitic drugs/meat分类
化学化工引用本文复制引用
罗辉泰,谢梦婷,黄晓兰,吴惠勤,朱志鑫,黄芳,林晓珊,欧阳钢锋..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[J].色谱,2015,(4):354-362,9.基金项目
广州市科技计划项目（11BppZXcc6100034）． （）
