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| Analysis of Ochratoxin A in Wine by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry with Stable Isotope Direct Dilution |
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| DOI： |
| KeyWord:stable isotope direct dilution ultra high performance liquid chromatography-tandem mass spectrometry wine ochratoxin A |
| Author | Institution |
| WANG Xing-long,CAI Qiang,GUI Wen-feng,CAI Zeng-xuan,XU Jiao-jiao,REN Yi-ping |
1.Analysis and Test Center,Yangtze Delta Region Institute of Tsinghua University，Zhejiang;2.School of Environmental and Geographical Sciences，Shanghai Normal University;3.Zhejiang Provincial Center for Disease Control and Prevention |
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| Abstract: |
| An ultra high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the determination of ochratoxin A(OTA) in wine based on stable isotope direct dilution technique.Samples were diluted with acetonitrile-water-formic acid(298∶70∶0.2,by volume),and the matrix effects were efficiently compensated with the 13C20-labelled internal standard.The analyte was separated on an ACQUITY BEH C18 column(100 mm×2.1 mm,1.7 μm) by gradient elution with 0.1% formic acid solution and 0.1% formic acid acetonitrile as mobile phases,and then analyzed under multiple reaction monitoring(MRM) mode in ESI+ mode.Results showed that there was a good linearity for OTA in the range of 0.05-1 μg/L with a correlation coefficient(r2) of 0.999 6.The limit of detection(LOD,S/N≥3) and the limit of quantitation(LOQ,S/N≥10) of the method were 0.1 μg/L and 0.3 μg/L,respectively.Recoveries at three spiked levels of 1.00,2.00,5.00 μg/L ranged from 102% to 113%,with intra day RSDs and inter day RSDs of 4.1%-9.4% and 4.4%-9.7%,respectively.The method was applied in the analysis of OTA in fifteen red wines and five white wines made in China,and OTA was undetected in all wines.The method was simple,effective and low-consumption,and was suitable for the determination of OTA in wine. |
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