15-acetyldeoxynivalenol and HT-2-toxin

In this report, a UPLC-ESI-MS/MS method for the simultaneous determination of aflatoxins, ochratoxin A, zearalenone, deoxynivalenol, fumonisins, T-2 and HT-2 toxins, fusarenone X, diacetoxyscirpenol, and 3- and 15-acetyldeoxynivalenol in feedstuffs was developed. A quadrupole-time-of-flight mass spectrometer detector (QTOF-MS) operating in full scan mode was combined with the UPLC-ESI-MS/MS system to confirm the identity of detected mycotoxins and to identify other possible microbial metabolites occurring in samples. Sixty-two feed samples from the Spanish market were analyzed. Extraction of metabolites was carried out with acetonitrile-water-formic acid (80:19:1, v/v/v). Method detection and quantification limits and performance criteria set by Commission Regulation (EC) No 401/2006 were fulfilled. Relatively high levels of the main regulated mycotoxins and presence of non-regulated mycotoxins in feed samples were found. This is the first study in which mycotoxins and other microbial metabolites occurring in feed are studied using a UPLC-QTOF-MS system being therefore a reference report.

Topics: Aflatoxins; Animal Feed; Chromatography, High Pressure Liquid; Fumonisins; Mass Spectrometry; Mycotoxins; Ochratoxins; T-2 Toxin; Trichothecenes; Zearalenone

A new, rapid and sensitive method is reported for the multiresidual determination of type A (diacetoxyscirpenol, HT-2 toxin, T-2 toxin) and type B (nivalenol, deoxynivalenol, fusarenon X, 15-O-acetyl-4-deoxynivalenol) trichothecenes in wheat flour samples. Sample extraction was performed with acetonitrile/water mixtures. Mycosep columns were used for a fast and effective clean-up procedure. The analytes were separated by HPLC with a RP C18 column by means of a gradient elution and detected in an ESI-interfaced single quadrupole mass spectrometer. Type B and type A trichothecenes were monitored in the negative and in the positive ion mode, respectively. The method performance is reported in terms of linearity (r2 = 0.999), specificity, accuracy (recoveries from 70-120%) and precision (CV% = 5), the LOQs are in the range 10-20 microg/Kg.

Topics: Chromatography, High Pressure Liquid; Drug Residues; Flour; Food Contamination; Mycotoxins; Reproducibility of Results; Spectrometry, Mass, Electrospray Ionization; T-2 Toxin; Trichothecenes; Triticum