Determination of Patulin in Fruit Products by Isotope Dilution Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry
  
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KeyWord:patulin  high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)  isotope dilution  fruit products
  
AuthorInstitution
XIANG Yu-zhi,XU Jiao-jiao,CAI Zeng-xuan,MO Wei-min,REN Yi-ping* 1.浙江工业大学化学工程学院;2.浙江省疾病预防与控制中心
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Abstract:
      A method was developed for the determination of patulin in fruit products by isotope dilution with high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).The clear juice was directly purified and enriched with ProElut PXA.Besides,the cloud juice,solid liquid and solid samples were primarily hydrolyzed with pectinase,then extracted with ethyl acetate and concentrated,redissolved with acetic acid solution(pH 4.0),and purified and enriched with ProElut PXA.The chromatographic separation was performed on a Waters HSS T3 column(2.1 mm×100 mm,1.8 μm) by gradient elution with acetonitrile-water as mobile phase.The patulin was detected by MS with electrospray negative ionization(ESI) under multiple reaction monitoring(MRM) mode.Accurate determination was achieved using isotope as the internal standard.Results showed that the calibration curve of patulin was linear in the range of 5-250 ng/mL with correlation coefficients greater than 0.999.The limits of quantitation(LOQ) of this method were 2.0 μg/kg for apple juice and 5.0 μg/kg for apple wine and haw.The recoveries of patulin at low,medium and high spiked concentration levels were in the range of 90.6%-110.1% with relative standard deviations of 1.4%-3.9%.The proposed method was proved to be a practical method which could completely satisfy the standard requirement GB 2761-2011 for detection of patulin in fruit products including apple juice,apple wine and haw products.In conclusion,this method was reliable,accurate and sensitive,and could be used for the analysis of patulin in fruit products.
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