| 稳定同位素直接稀释/超高效液相色谱-串联质谱法测定葡萄酒中赭曲霉毒素A |
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| 基金项目:国家重点研发计划(2017YFC1601300) |
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| 中文摘要:建立了稳定同位素直接稀释/超高效液相色谱-串联质谱(UPLC-MS/MS)测定葡萄酒中赭曲霉毒素A(OTA)的方法。葡萄酒样品经乙腈-水-甲酸(298∶70∶0.2，体积比)溶液稀释后，加入稳定同位素消除基质效应的影响。采用ACQUITY BEH C18色谱柱(100 mm×2.1 mm，1.7 μm)分离，以0.1%甲酸水-0.1%甲酸乙腈为流动相梯度洗脱，以电喷雾离子源正离子模式(ESI+)扫描，多反应监测(MRM)模式采集，内标法定量。结果表明，OTA在0.05~1 μg/L范围内线性关系良好，相关系数(r2)为0.999 6，检出限(LOD,S/N≥3)为0.1 μg/L，定量下限(LOQ,S/N≥10)为0.3 μg/L。在1.00、2.00、5.00 μg/L加标水平下，回收率为102%~113%，日内相对标准偏差(RSD)为4.1%~9.4%，日间RSD为4.4%~9.7%。利用该方法对国产品牌的15种红葡萄酒和5种白葡萄酒进行测定，均未检出OTA。此方法简单、高效、节约成本，可用于大批量葡萄酒中OTA的快速、准确检测。 |
| 中文关键词:稳定同位素 直接稀释 超高效液相色谱－串联质谱 葡萄酒 赭曲霉毒素A |
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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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| 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. |
| Key Words:stable isotope direct dilution ultra high performance liquid chromatography-tandem mass spectrometry wine ochratoxin A |
| 引用本文：王兴龙,蔡强,桂文锋,蔡增轩,许娇娇,任一平.稳定同位素直接稀释/超高效液相色谱-串联质谱法测定葡萄酒中赭曲霉毒素A[J].分析测试学报,2019,38(11):1379-1383. |
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