Determination of Ochratoxin A in Wine by Immunoaffinity Cleanup and Liquid Chromatography Tandem Mass Spectrometry

Abstract

A simple and accurate method has been developed for determining ochratoxin A (OTA), using an immunoaffinity column for cleanup and liquid chromatography-tandem mass spectrometry for identification and quantification. Wine samples were diluted with a solution containing polyethylene glycol 8000 and sodium hydrogen carbonate, filtered through a glass microfiber filter, and cleaned up on an immunoaffinity column. OTA was then eluted with methanol-acetic acid (98:2) and analyzed by liquid chromatography-tandem mass spectrometry. The average recoveries of OTA from red and white wines were 95 and 96.7% (spiked OTA level was 0.05 ng/ml) and repeatabilities (relative standard deviation) were 3.8 and 2.4%, respectively. The detection limit was 0.0003 ng/ml based on the signal-to-noise ratio in wine of 3:1. Analysis of 74 samples of domestic and imported wines showed OTA levels ranging from < 0.0003 to 0.82 ng/ml, with an incidence of contamination of 92.1% for red wines, and < 0.0003 to 0.51 ng/ml, with an incidence of contamination of 77.8% for white wines. These detection rates were higher than those rates of past reports of OTA contamination in wine, due to the high sensitivity of this method. However, all samples analyzed in this study complied with European Union regulations. It is concluded that this method is a useful tool for the quality assurance of wine.

Determination of ochratoxin a in wine by high-performance thin-layer chromatography using charged coupled device

“…These results of validation were similar to those of the official method used to determine ochratoxin in wine, which found average recoveries from wine samples spiked at levels from 0.04 to 10 μg L -1 ranging from 88% to 103% and the detection limit was 0.01 μg L -1 using immunoaffinity column clean-up and HPLC. 6 Noba et al 42 developed a method based in the use of immunoaffinity column for clean-up . The repeatabilities expressed as relative standard deviation were 3.8 and 2.4%, respectively.…”

“…25,27,[42][43][44][45][46] In Brazil, Rosa et al 47 analyzed 80 samples of national and imported wines. OTA were detected in 28.75% of samples, at concentrations ranging from 0.021 to 0.071 μg L More studies must be conducted on OTA occurrence in wines and grape juices produced in Brazil.…”

An electrochemical immunosensor for ochratoxin A determination in wines based on a monoclonal antibody and paramagnetic microbeads

“…HPLC with mass spectrometry detection (HPLC-MS) has also been proposed for the determination of OTA in wine and beer samples (LODs of about 0.003 ng mL −1 and measurement ranges of 0.01 to 1 ng mL −1 of OTA) [9][10][11].…”

A Method for Multiple Mycotoxin Analysis in Wines by Solid Phase Extraction and Multifunctional Cartridge Purification, and Ultra-High-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry

“…This is the lowest regulatory level for mycotoxins with the exception of aflatoxin, for which a tolerable intake is not established, because of their genotoxic effects. The occurrence of OTA in wine has been reported in several studies [3,4,5,6,7], and several countries have their own regulations to control OTA in wine products; for instance, its maximum level established by the European Union (EU) is 2 μg/L [8]. A recent study also reports the occurrence of fumonisins (FMs), in particular FMB2, in red wine [9].…”