Determination of mycotoxins in different food commodities by ultra‐high‐pressure liquid chromatography coupled to triple quadrupole mass spectrometry

Abstract

A rapid multianalyte-multiclass method with little sample manipulation has been developed for the simultaneous determination of eleven mycotoxins in different food commodities by using ultrahigh-pressure liquid chromatography coupled to triple quadrupole mass spectrometry (UHPLC/MS/ MS). Toxins were extracted from the samples with acetonitrile/water (80:20, v/v) 0.1% HCOOH and, after a two-fold dilution with water, directly injected into the system. Thanks to the fast highresolution separation of UHPLC, the eleven mycotoxins were separated by gradient elution in only 4 min. The method has been validated in three food matrices (maize kernels, dry pasta (wheat), and eight-multicereal babyfood (wheat, maize, rice, oat, barley, rye, sorghum, millet)) at four different concentration levels. Satisfactory recoveries were obtained (70-110%) and precision (expressed as relative standard deviation) was typically below 15% with very few exceptions. Quantification of samples was carried out with matrix-matched standards calibration. The lowest concentration successfully validated in sample was as low as 0.5 mg/kg for aflatoxins and ochratoxin A in babyfood, and 20 mg/kg for the rest of the selected mycotoxins in all matrices tested. Deoxynivalenol could be only validated at 200 mg/kg, due the poor sensitivity for this mycotoxin analysis. With only two exceptions (HT-2 and deoxynivalenol), the limits of detection (LODs), estimated for a signal-to-noise ratio of 3 from the chromatograms of samples spiked at the lowest level validated, varied between 0.1 and 1 mg/kg in the three food matrices tested. The method was applied to the analysis of different kinds of samples. Positive findings were confirmed by acquiring two transitions (Q quantification, q confirmation) and evaluating the Q/q ratio.

Determination of aflatoxins B1, B2, G1, G2 and ochratoxin A in animal feed by ultra high‐performance liquid chromatography–tandem mass spectrometry

“…For that purpose, UHPLC is a technique that offers advantages, such as better sensitivity, resolution and speed of analysis than LC [30], because of the use of columns filled with sub 2 mm particle size. Despite of the advantages of UHPLC, up to now there have been few published studies that determine mycotoxins in several matrices [5,[31][32][33].…”

High Throughput Detection Methods for Multiplex Mycotoxins

“…Mycosep ® /Multisep ® purification are another well-established method for multiplex mycotoxins. Mycosep ® #226 and #227 were often used for purification for multiplex mycotoxin analysis [30,32,38,50,62]. These columns comprise different adsorbents (e.g., charcoal and ionexchange resins), which can adsorb proteins, fats and pigments of samples no requirement for activation, washing and elution.…”

Comparison of approaches to deal with matrix effects in LC-MS/MS based determinations of mycotoxins in food and feed

“…The selection of the matrices was based on the moderate to strong signal suppression associated with these types of matrices. Maize was chosen as the least complex matrix in this work, but its relative high matrix effects have been widely described (Beltran et al, 2009;De Girolamo et al, 2013).…”