Journal of AOAC International 2006-01-01

Residue determination of captan and folpet in vegetable samples by gas chromatography/negative chemical ionization-mass spectrometry.

Mercedes Barreda, Francisco J López, Mercedes Villarroya, Joaquim Beltran, Jose María García-Baudín, Felix Hernández

Index: J. AOAC Int. 89(4) , 1080-7, (2006)

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Abstract

A gas chromatography/negative chemical ionization-mass spectrometry (GC/NCI-MS) method has been developed for the simultaneous determination of the fungicides captan and folpet in khaki (persimmon; flesh and peel) and cauliflower. Samples were extracted with acetone in the presence of 0.1 M zinc acetate solution in order to avoid degradation of fungicides and were purified using solid-phase extraction with divinylbenzene polymeric cartridges. Purified extracts were evaporated and dissolved in hexane prior to injection into the GC/NCI-MS system. Isotope-labeled captan and folpet were used as surrogate/internal standards, and quantification was performed using matrix-matched calibration. The method showed linear response in the concentration range tested (50-2500 ng/mL). The method was fully validated with untreated blank samples of khaki (flesh and peel) and cauliflower spiked at 0.05 and 0.5 mg/kg. Satisfactory recoveries between 82 and 106% and relative standard deviations lower than 11% in all cases (n = 5) were obtained. The limit of detection for both compounds were estimated to be 0.01 mg/kg. The developed method has been applied to treated and untreated samples collected from residue trials.