Dispersive Solid-phase Extraction Followed by Liquid Chromatography-Tandem Mass Spectrometry for Rapid Determination of 87 Kinds of Drug Residues in Feedingstuffs
  
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KeyWord:dispersive solid-phase extraction(dSPE)  high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)  dynamic multiple reaction ion monitoring(dMRM)  feedingstuffs  β-agonists  coccidiostats  antibiotics
  
AuthorInstitution
LUO Hui-tai,HUANG Xiao-lan*,WU Hui-qin,ZHONG Qiao-li,ZHU Zhi-xin,HUANG Fang, LIN Xiao-shan,XIE Meng-ting,OUYANG Gang-feng 1.中国广州分析测试中心广东省化学危害应急检测技术重点实验室;2.中山大学化学与化学工程学院
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Abstract:
      A generic,rapid and simple multiresidue analytical method was developed and validated for determination of 8 classes of drugs including 17 β-agonists,18 β-lactams,6 coccidiostats,5 macrolides,2 lincosamides,15 quinolones,21 sulfonamides and 3 sulfonamides potentiators in feedingstuffs using dispersive solid-phase extraction(dSPE) method and high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The homogenized sample was dispersed by 0.1 mol/L Na2EDTA solution,the analytes were extracted with a mixture of methanol-acetonitrile(50∶50) by ultrasonic,and then the extracts were purified by dispersive solid phase extraction using Bondesil-PSA as adsorbent.Electrospray ionization mass spectrometry was operated in the positive mode using dynamic multiple reaction monitor(dMRM) for the qualitative and quantitative analysis of 87 kinds of analytes after the separation on a Poroshell EC-C18(100 mm×2.1 mm,2.4 μm) column.The correlation coefficients of linear calibration curves were over 0.99 in the corresponding concentration range.The average recoveries of 87 drugs at three different spiked concentration levels ranged from 63.7% to 108.8%,with relative standard deviations(RSDs) of 3.5%-15.2%.The limits of detection(LODs,S/N≥3) and quantitation(LOQs,S/N≥10) were 3-15 μg/kg and 10-50 μg/kg,respectively.The method was simple,rapid,sensitive and reliable,and was suitable for the determination of residues in feedingstuffs.
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