Compensation for matrix effects in gas chromatography-tandem mass spectrometry using a single point standard addition
JOURNAL OF CHROMATOGRAPHY A
Authors: Garrido Frenich, Antonia; Martinez Vidal, Jose Luis; Fernandez Moreno, Jose Luis; Romero-Gonzalez, R.
Abstract
One of the major problems in quantitative analysis of pesticide residues in food samples by gas chromatography-tandem mass spectrometry (GC-MS/MS) is the enhancement or the suppression, of the target analyte signals in matrix extracts. Potentially positive samples, which had previously been identified by a rapid screening method, were quantified using standard addition to compensate matrix effects. As example we performed a systematic study on the application of the standard addition calibration (SAC) method for the determination of 12 pesticides (acephate, bromopropylate, chlorpyrifos, cypermethrin, diazinon, etrimfos, heptenophos, iprodione, methamidophos, procymidone, tetradifon, and triadimefon) in two matrices (cucumber and orange) in the range of initial concentrations of 10-200 mu g kg(-1). The influence of some factors, such as the minimum number of standard additions used (single, two, three or four points calibration), as well as the known amount of analyte added to the sample, is evaluated in order to obtain reliable results. Accurate quantification is achieved when a single point SAC at 200 mu g kg(-1) was used. obtaining for all the cases recoveries between 70 and 120%. The proposed analytical approach only needs two injections per sample (blank and spiked extracted sample) to determine the final concentration of pesticide in positive samples. (C) 2009 Elsevier B.V. All rights reserved.
Fumonisin B-1 and zearalenone contamination of wheat in Croatia and influence of fungicide treatments
PHYTOPROTECTION
Authors: Ivic, Dario; Domijan, Ana-Marija; Peraica, Maja; Cvjetkovic, Bogdan
Abstract
In Croatia, a trial was conducted to determine the presence of the Fusarium mycotoxins fumonisin B, and zearalenone in wheat kernels and to evaluate the efficacy of nine fungicides on Fusarium head blight severity as well as fumonisin B-1 and zearalenone accumulation in wheat grain. Fumonisin B-1 and zearalenone were detected in all grain samples in mean concentrations ranging from 182.0 to 446.6 mu g kg(-1) (fumonisin B-1) and from 2.59 to 5.33 mu g kg(-1) (zearalenone). No significant differences were found among fumonisin B-1 and zearalenone content in wheat grain for the different fungicide treatments. No correlation was revealed between Fusarium head blight severity and fumonisin B-1 or zearalenone content in wheat grain, nor between fungicide efficacy and fumonisin B-1 or zearalenone content in wheat grain. Under conditions of high disease pressure, efficacy of the fungicides was between 85.7% (tebuconazole + triadimefon) and 72.1% (carbendazim).