Automated On-line Solid-Phase Extraction−Liquid Chromatography−Electrospray Tandem Mass Spectrometry Method for the Determination of Ochratoxin A in Wine and Beer

Abstract

An automated on-line solid-phase extraction-liquid chromatography-electrospray tandem mass spectrometry (SPE-LC-ESI-MS/MS) method was developed for the determination of ochratoxin A (OTA) in alcoholic beverages. Mean recoveries for wine and beer were, respectively, 75 and 82%. Detection was achieved in negative ionization with a Q TRAP mass spectrometer operating in multiple-reaction monitoring (MRM) mode or enhanced product ion (EPI) mode, using the third quadrupole as linear ion trap. The MRM mode turned out to be more sensitive; the method allowed accurate determination of OTA in the range of 0.01-25 ng mL(-1) using external calibration. Within-day and between-day relative standard deviation percentages were <6.2 and <9.1%, respectively. In EPI mode, fragmentation spectra at the limit of quantification (0.03 ng mL(-1)) and good linearity could be obtained. Application of the method (MRM mode) to the analysis of several wine and beer samples purchased in local stores revealed OTA levels in the ranges of 0.03-1.44 ng mL(-1) for wines and 0.02-0.14 ng mL(-1) for beers.

Mycotoxin Contamination of Beverages: Occurrence of Patulin in Apple Juice and Ochratoxin A in Coffee, Beer and Wine and Their Control Methods

“…In Italy, Visconti et al [147] found OTA in 30 out of 61 beer samples, with no substantial differences between strong and light beers. The results of Bacaloni et al [148] agreed with these data. In Germany, the first results were obtained with methods having a relatively high limit of detection, so consequently, the frequency of positive samples (42.5%) was low, although values as high as 1.53 ng/mL were reported.…”

Combination of On-Line Solid-Phase Extraction with LC-MS for the Determination of Potentially Hazardous Glycoalkaloids in Potato Products

“…As m/z 98.2 emerged in both fragmentation scans with the highest intensity, we chose it as the identification ion. At present, chromatographic separation followed by MRM detection of two ions can be used to precisely identify a molecule (Bacaloni et al 2005).…”

“…Only a few methods have been developed for the analysis of food ingredients so far. Bacaloni et al (2005), as well as Newkirk et al (1998), investigated mycotoxins in wine, beer and corn-based feed. In nutraceuticals, ephedrine could be detected with automated SPE-HPLC (Stevens 2003).…”

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].…”