Determination of 46 Antibiotics Residues in Organic Fertilizer by UPLC-MS/MS with QuEChERS Combined with Column Purification
  
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KeyWord:ultrahigh performance liquid chromatography-tandem massspectrometry(UPLC-MS/MS)  antibiotics residues  organic fertilizer  QuEChERS combined with column purification
  
AuthorInstitution
WANG Jian-mei,LIU Yan-ping,CHEN Jing,WU Hui-zhen,XIA Wei,LI Zu-guang,QIAN Ming-rong* 1.浙江省农业科学院农产品质量标准研究所,浙江省植物有害生物防控重点实验室-省部共建国家重点实验室培育基地;2.浙江工业大学化工学院;3.浙江医药股份有限公司
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Abstract:
      A confirmative method was developed for the simultaneous determination of 46 antibiotics,including sulfonamides,quinolones and macrolides in organic fertilizer by ultrahigh performance liquid chromatography-tandem massspectrometry(UPLC-MS/MS).The samples were extracted with acetonitrile-EDTA buffer solution(pH 10.0),and separated by centrifugation after salting out.The upper acetonitrile layer was purified by the QuEChERS steps with sorbents.The buffer solution layer was purified with solid-phase extraction cartridge.The separation of target drugs was performed on an ACQUITY UPLC BEH C18column using a mobile phase consisting of 2 mmol/L ammonium acetate with 0.1% formic acid and methanol by gradient elution.The analysis of target compounds was carried out with positive electrospray ionization(ESI+)source under multiple reaction monitoring(MRM) mode.The matrix-matched external standard calibration was used for quantification.Good linearities for the 46 antibiotics were achieved over the concentration of 1-200 μg/L,with correlation coefficients(r2) of 0.996 6-0.999 9.The recoveries of sulfonamides,quinolones and macrolides at spiked levels of 25,100,400 μg/kg were in the range of 67.8%-95.6%,65.6%-89.4% and 66.6%-107.8%,respectively,with relative standard deviations(RSDs) of 0.4%-11.9%.The limits of detection(LOD,S/N=3) were 0.6-4.6 μg/kg,and the limits of quantitation(LOQ,S/N=10) were 2.1-15.4 μg/kg.
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