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

Abstract

An analytical method using two solid phase extractions and ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was developed for the identification and quantification of 14 mycotoxins (patulin, deoxynivalenol, aflatoxins B1, B2, G1, G2, M1, T-2 toxin, HT-2 toxin, zearalenone, fumonisins B1, B2, B3, and ochratoxin A) in domestic and imported wines. Mycotoxins were purified with an Oasis HLB cartridge, followed by a MultiSepTM #229 Ochra. As a result, sufficient removal of the pigments and highly polar matrices from the red wines was achieved. UHPLC conditions were optimized, and 14 mycotoxins were separated in a total of 13 min. Determinations performed using this method produced high correlation coefficients for the 14 mycotoxins (R > 0.990) and recovery rates ranging from 76 to 105% with good repeatability (relative standard deviation RSD < 12%). Twenty-seven samples of domestic and imported wines were analyzed using this method. Although ochratoxin A (OTA) and fumonisins (FMs) were detected in several samples, the FM levels were less than limits of quantification (LOQs) (1 μg/L), and even the largest of the OTA levels was below the EU regulatory level (2 μg/L). These results suggest that the health risk posed to consumers from the wines available in Japan is relatively low.

Developments in the Monitoring of Patulin in Fruits Using Liquid Chromatography: an Overview

“…LOQ for patulin was 5 μg L −1 with recoveries of 78% (Tamura et al 2012). To overcome sensitivity drawback, several single-target LC-MS methods that employed more sophisticated sample pre-treatment have been proposed for patulin quantification.…”

“…The mobile phase composed of water and methanol or water and acetonitrile with addition of acetic acid (Tamura et al 2012;Hammami et al 2017) or ammonium acetate (Christensen et al 2009;Malachová et al 2014;Seo et al 2015;Vaclavikova et al 2015) is used for this mycotoxin analysis. Unfortunately, due to high polarity of target molecule, the LC-MS analysis suffers from low sensitivity.…”

“…This approach allows for isolation, concentration, as well as purification of target molecule. SPE has been appreciated by researchers studying patulin contamination in variety of fruit products (juices, purees, jams) and was used separately (Li et al 2007b;Funes and Resnik 2009;Catana et al 2011;Zhou et al 2012) or in combination with liquid-liquid extraction (Spadaro et al 2008;Barreira et al 2010;Zaied et al 2013;Karakose et al 2015;Seo et al 2015;De Clercq et al 2016) (Tamura et al 2012). Nevertheless, like any other technique, SPE has also some limitations.…”

“…The improvements in matrix compounds separation could be achieved by introduction of buffering salts (sodium citrate, sodium hydrogen citrate sesquihydrate) into traditional mixture of magnesium sulfate anhydrous and sodium chloride for better pH control and improved recovery rate (Marsol-Vall et al 2014;Sadok et al 2018). The purification step is performed using dSPE (Desmarchelier et al 2011;Marsol-Vall et al 2014;Sadok et al 2018) and rarely by traditional SPE columns (Tamura et al 2012).…”

“…QuEChERS methodology has been recently applied for patulin determination in different fruits: apples, pears, peaches, apricots, bananas, strawberries, grapes, plums, raspberries, blackberries, blueberries, sour cherries (Anastassiades et al 2003;Desmarchelier et al 2011;Marsol-Vall et al 2014;Sadok et al 2018;Vaclavikova et al 2015;Tamura et al 2012). …”