Experimental Techniques and MethodsSimultaneous Determination of Kasugamycin and Benziothiazolinone Residues in Citrus by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid Phase Extraction
  
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KeyWord:dispersive solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  citrus  kasugamycin  benziothiazolinone
  
AuthorInstitution
AN Jiao,KANG Xia-li,YANG Qin,ZHAO Qi-yang,ZHANG Yao-hai,WANG Cheng-qiu,JIAO Bi-ning Quality Supervision and Testing Center for Citrus and Seedling,Ministry of Agriculture and Rural Affairs,Laboratory of Risk Assessment for Citrus Quality and Safety,Citrus Research Institute,Southwest University/Chinese Academy of Agricultural Sciences
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Abstract:
      An analytical method was developed for the simultaneous determination of kasugamycin and benziothiazolinone residues in citrus by dispersive solid phase extraction/ultra performance liquid chromatography-tandem mass spectrometry(DSPE/UPLC-MS/MS).Citrus whole fruit and pulp were extracted with acetonitrile containing 0.5% formic acid and 0.5% aqueous ammonia-water(7∶3,by volume),respectively,then purified with octadecyl silica gel(C18) and separated on a Waters ACQUITY UPLC HSS T3 column by gradient elution with 0.2% aqueous formic acid-methanol as mobile phase,finally analyzed in multiple reaction monitoring(MRM) mode and quantified by matrix matched standard curve external standard method.Results showed that there were good linear relationships for the target compounds in the range of 0.5-200 μg/L with their correlation coefficients(r2) larger than 0.999.The limits of detection(LODs) and the limits of quantitation(LOQs) were in the concentration ranges of 0.006-0.04 μg/kg and 5-10 μg/kg,respectively.The spiked recoveries ranged from 73.4% to 104% with relative standard deviations(RSDs,n=6) of 1.6%-96%.With easy operation and high sensitivity,the method is suitable for the simultaneous determination of kasugamycin and benziothiazolinone residues in citrus.
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