Determination of 15 Mycotoxins in Dry-cured Hams with QuEChERS-based Extraction and Liquid Chromatography-Tandem Mass Spectrometry
  
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DOI:10.3969/j.issn.1004-4957.年份.月份
KeyWord:dry-cured ham  mycotoxins  liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)  dispersive solid phase extraction  QuEChERS
  
AuthorInstitution
GUO Li-qiang*,GONG Xiao-ming,DING Kui-ying,WANG Ke,SUN Jun,ZHAO Han 1.潍坊出入境检验检疫局;2.石家庄市疾病预防控制中心
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Abstract:
      A method was developed for the simultaneous determination and identification of 15 mycotoxin residues in dry-cured hams,including aflatoxin B1,aflatoxin B2,aflatoxin G1,aflatoxin G2,ochratoxin A,citrinin,T-2 toxin,HT-2 toxin,diacetoxyscirpenol,neosolaniol,verruculogen,O-methyl sterigmatocystin,sterigmatocystin,cyclopiazonic acid and penicillic acid,by liquid chromatography-tandem triple-quadrupole linear ion trap mass spectrometry(LC-MS/MS).The dry cured ham samples were purified by QuEChERS method after extraction with acetonitrile solution containing 1% formic acid,then separated on an Eclipse Plus C18 column(3.0 mm×100 mm,1.8 μm) by gradient elution with mobile phases of 5 mmol/L ammonium acetate aqueous solution(containing 0.1% formic acid and 9.9% acetonitrile,A) and acetonitrile(containing 0.1% formic acid,B).A multiple reaction monitoring(MRM) as survey scan and an enhanced product ion(EPI) scan as dependent scan were performed in an information dependent acquisition(IDA) experiment.The identification of compounds was carried out by library search with a newly developed MS/MS library based on EPI spectra in positive mode.The results showed that the calibration curves were linear in the range of 0.05-200 μg/L for 15 mycotoxins with correlation coefficients(r) more than 0.993.The limits of quantitation(LOQs,S/N=10) were in the range of 0.05-2.5 μg/kg.The average recoveries(n=6) of 15 mycotoxins in dry-cured ham samples at three spiked levels(1 times,2 times,10 times of LOQ) ranged from 79.1% to 95.5% with relative standard deviations(RSDs) of 3.2%-12.8%.The method was sensitive,convenient and accurate,and could satisfy the demand for detection of mycotoxin residues in contaminated dry-cured meat.
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