Determination of Ochratoxin A and Ochratoxin B in Archived Tokaj Wines (Vintage 1959-2017) Using On-Line Solid Phase Extraction Coupled to Liquid Chromatography.

Aneta Kholová,Andrea Machyňáková,Ivona Lhotská,Petr Solich,Dalibor Šatínský,František Švec,Ivan Špánik,Adéla Uhrová

doi:10.3390/toxins12120739

Aneta Kholová, Andrea Machyňáková + Show 6 more

Open Access

https://doi.org/10.3390/toxins12120739

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Abstract

According to the EU legislation, ochratoxin A contamination is controlled in wines. Tokaj wine is a special type of sweet wine produced from botrytized grapes infected by “noble rot” Botrytis cinerea. Although a high contamination was reported in sweet wines and noble rot grapes could be susceptible to coinfection with other fungi, including ochratoxigenic species, no screening of Tokaj wines for mycotoxin contamination has been carried out so far. Therefore, we developed an analytical method for the determination of ochratoxin A (OTA) and ochratoxin B (OTB) involving online SPE coupled to HPLC-FD using column switching to achieve the fast and sensitive control of mycotoxin contamination. The method was validated with recoveries ranging from 91.6% to 99.1% with an RSD less than 2%. The limits of quantification were 0.1 and 0.2 µg L−1 for OTA and OTB, respectively. The total analysis time of the online SPE-HPLC-FD method was a mere 6 min. This high throughput enables routine analysis. Finally, we carried out an extensive investigation of the ochratoxin contamination in 59 Slovak Tokaj wines of 1959–2017 vintage. Only a few positives were detected. The OTA content in most of the checked wines did not exceed the EU maximum tolerable limit of 2 µg L−1, indicating a good quality of winegrowing and storing.

Highlights

Ochratoxins belong to the group of mycotoxins that are secondary metabolites produced by fungal species growing on plants and plant products with toxic effects on humans and animals [1]
We focused on the optimization of a method that enables the fast extraction of mycotoxins from the wine with a high recovery
Official AOAC method using immunoaffinity clean-up, we achieved the full automation of the the Official AOAC method using immunoaffinity clean-up, we achieved the full automation of the extraction process coupled to chromatographic analysis with the same limit of quantification for ochratoxin A (OTA), extraction process coupled to chromatographic analysis with the same limit of quantification for

Summary

Introduction

Ochratoxins belong to the group of mycotoxins that are secondary metabolites produced by fungal species growing on plants and plant products with toxic effects on humans and animals [1]. Ochratoxin A (OTA) is the most common and widespread ochratoxin found in a wide variety of agricultural commodities worldwide, ranging from cereal grains to dried fruits and spices to wine, coffee, and cocoa [1,2]. A is classified as a possible human carcinogen (Group 2B) by the International Agency for Research on Cancer [3]. The less common ochratoxin B (OTB), a non-chlorinated OTA analog, is less toxic than OTA [7,8]. OTB contamination exceeding OTA levels was found in several red wines from Italy and Spain [9,10]. The European Food Safety Authority set the tolerable weakly intake of OTA at 120 ng per kg body weight, and the European Commission established the maximum permitted OTA content in wine at 2 μg kg−1 [11]

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