Determination of Ochratoxin A in Grapes, Dried Vine Fruits, and Winery Byproducts by High-Performance Liquid Chromatography with Fluorometric Detection (HPLC−FLD) and Immunoaffinity Cleanup

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• 作者：Michele Solfrizzo ; Giuseppe Panzarini ; Angelo Visconti
• 刊名：Journal of Agricultural and Food Chemistry
• 出版年：2008
• 出版时间：December 10, 2008
• 年：2008
• 卷：56
• 期：23
• 页码：11081-11086
• 全文大小：160K
• 年卷期：v.56,no.23(December 10, 2008)
• ISSN：1520-5118

文摘

A liquid chromatographic method for the determination of ochratoxin A in grapes, dried vine fruits, and winery byproducts was developed. A mixture of either acetonitrile/water or acetonitrile/water/methanol was used as an extraction solvent mixture. After immunoaffinity column cleanup, the final extract was analyzed by high-performance liquid chromatography (HPLC) with a fluorometric detector (FLD). Mean recoveries from grapes, grape pomace, and lees samples spiked in the range of 1−200 μg/kg were 78, 86, and 88%, respectively, with a detection limit of 0.1 μg/kg and within-laboratory repeatability ranging from 6 to 15%. Tested on naturally contaminated samples of grapes, grape pomace, and sultanas, the method showed better performances as compared to two other methods also based on immunoaffinity cleanup and HPLC/FLD determination. Ochratoxin A was detected in samples of grape pomace (levels ranging from 34.2 to 456.8 μg/kg) and lees (levels ranging from 48.3 to 602.5 μg/kg) derived from the wine making of red grapes of 2004 and 2005 vintages in southern Italy. After distillation of contaminated grape pomace in a pilot-scale equipment to produce grappa, the toxin remained unchanged in the exhausted pomace and was not detected in any of the distilled fractions (detection limit of 0.02 μg/L).