Liquid chromatography/tandem mass spectrometry for the identification and determination of trichothecenes in maize

Abstract

A reliable, sensitive and selective liquid chromatography/tandem mass spectrometry (LC/MS/MS) method has been developed to determine four trichothecene mycotoxins (nivalenol, deoxynivalenol, fusarenon X and 3-acetyldeoxynivalenol) in maize. Sample preparation was performed by extracting the analytes with a mixture of acetonitrile and water, followed by a solid-phase extraction with Carbograph-4 cartridges as the purification step. For the LC/MS/MS analysis two interfacing systems, Turbo IonSpray (TISP) and atmospheric pressure chemical ionization (APCI), were compared in both negative and positive ion modes. LC and MS parameters were optimized to achieve better results and sensitivity. The effect of mobile phase modifiers such as ammonium acetate and formic acid on the ionization yield was also evaluated. The best results were obtained using the electrospray ionization (ESI) interface in negative ion mode and the multiple reaction monitoring mode (MRM) for the quantitation. The detection limits ranged between 10 ng/g for fusarenon X and 1.5 ng/g for deoxynivalenol. A linear working range was achieved with a standard deviation between 3 and 10% and recovery rates from the maize samples above 81%. The procedure was applied to the analysis of a set of maize samples collected from farms located in different areas of northern and central Italy. The investigated samples turned out to be contaminated primarily with deoxynivalenol and, to a minor extent, with its derivatives.

Development of a multicomponent method forFusariumtoxins using LC-MS/MS and its application during a survey for the content of T-2 toxin and deoxynivalenol in various feed and food samples

“…In accordance to literature data (RazzaziFazeli 1999(RazzaziFazeli , 2002Zö llner et al 1999;Lau et al 2000;Lagana et al 2003), electrospray with negative ionization proved to be applicable more widely than with positive ionization. Negatively charged molecular ions of type B-trichothecenes (NIV, DON, ADON, FX) were detected by far more sensitively than their positively charged analogues.…”

“…The comparison shows a six to 17 times higher response when the ESI interface is used. Lagana et al (2003) reported similar results for an older type of the API Instrument (API 365), while Berthiller et al (2005) received the best results using the APCI interface in combination with an ammonia acetate buffer.…”

“…Most common methods for simultaneous determination of A and B-trichothecenes require GC-ECD, GC-MS or LC with post-column derivatization and fluorescence detection (Krska 2001). Recently, LC-MS/MS has been increasingly applied to mycotoxin analysis (Berger et al 1999;Razzazi-Fazeli et al 1999, 2002Zö llner et al 1999;Lau et al 2000, Plattner 2000Lagana et al 2003;Pallaroni & Holst 2003;Royer et al 2004;Berthiller et al 2005). The main advantages are its general applicability, high sensitivity and outstanding selectivity.…”

Gas chromatography: mass spectrometry determination of trichothecene mycotoxins in commercial corn harvested in the state of São Paulo, Brazil

“…7,18,19 More recently some methods have been developed using the liquid chromatography/tandem mass spectrometry for identification and determination of trichothecenes type A and B. 20,21 Despite of this, GC-MS is specially appropriate for its capability for simultaneous detection of trichothecenes from the groups A and B and for providing unequivocal identification.…”

Recent advances in mycotoxin determination in food and feed by hyphenated chromatographic techniques/mass spectrometry

“…In a very recent study, the analysis of four type B trichothecenes (NIV, DON, FUSX, 3-ADON) was performed in maize by an LC/MS/MS technique, comparing the commonly used Atmospheric Pressure Chemical Ionization (APCI) interface to the TurboIonSpray (TISP) interface in both negative and positive ion modes (Laganà et al, 2003). The most valuable spectra for each trichothecene were obtained using the turbo ion spray TISP-ESI system in the negative ion mode, gradient elution from water/methanol/acetonitrile 90:3:7 to water/methanol/ acetonitrile 20:24:56, with no modifier.…”