Determination of Ochratoxin A in Wine and Beer by Immunoaffinity Column Cleanup and Liquid Chromatographic Analysis with Fluorometric Detection: Collaborative Study

Abstract

The accuracy, repeatability, and reproducibility characteristics of a liquid chromatographic method for the determination of ochratoxin A (OTA) in white wine, red wine, and beer were established in a collaborative study involving 18 laboratories in 10 countries. Blind duplicates of blank, spiked, and naturally contaminated materials at levels ranging from ≤0.01 to 3.00 ng/mL were analyzed. Wine and beer samples were diluted with a solution containing polyethylene glycol and sodium hydrogen carbonate, and the diluted samples were filtered and cleaned up on an immunoaffinity column. OTA was eluted with methanol and quantified by reversed-phase liquid chromatography with fluorometric detection. Average recoveries from white wine, red wine, and beer ranged from 88.2 to 105.4% (at spiking levels ranging from 0.1 to 2.0 ng/mL), from 84.3 to 93.1% (at spiking levels ranging from 0.2 to 3.0 ng/mL), and from 87.0 to 95.0% (at spiking levels ranging from 0.2 to 1.5 ng/mL), respectively. Relative standard deviations for within-laboratory repeatability (RSDr) ranged from 6.6 to 10.8% for white wine, from 6.5 to 10.8% for red wine, and from 4.7 to 16.5% for beer. Relative standard deviations for between-laboratories reproducibility (RSDR) ranged from 13.1 to 15.9% for white wine, from 11.9 to 13.6% for red wine, and from 15.2 to 26.1% for beer. HORRAT values were ≤0.4 for the 3 matrixes.

Detection of ochratoxin A andcis- andtrans-resveratrol in red wines and their musts from Calabria (Italy)

“…OTA analyses were performed according to the AOAC Official Method 2001.01 (Visconti et al 2001). Wine samples (20 ml) were diluted with 20 ml of a solution containing 1% polyethylene glycol (PEG 8000) and 5% sodium bicarbonate and filtered through glass microfiber filters.…”

BSA-based sample clean-up columns for ochratoxin A determination in wine: Method development and validation

“…The determination of OTA in wine by IAC followed the AOAC Official Method 2001.01 (Visconti, Pascale, & Centonze, 2001). Briefly, OTA-spiked wine samples prepared above (0.05, 0.5, 1, 2 and 3 µg L −1 ) were diluted 1:2 in 1% PEG 8000/5% NaHCO 3 pH 8.3 and filtered through a 1 µm glass microfiber syringe filter (Whatman).…”

Ochratoxin A and Brewing Technology: A Review

“…P. verrucosum primarily contaminates plants such as cereal crops, whereas P. nordicum has been primarily detected in meat products and cheese 63 . In tropical and semitropical regions, OTA is primarily produced by Aspergillus ochraceus 59,82,125 . A. ochraceus is also referred to as A. allutaceus var.…”

“…allutaceus 59 . A. ochraceus has been reported in a large variety of produce such as nuts, dried peanuts, beans, spices, green coffee beans and dried fruits, and also in processed meats and smoked and salted fish 125 . Two other species of Aspergillus section Nigri, respectively, A. niger var.…”