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A direct comparison with reverse-phase LC-MS/MS and GC-MS/MS was conducted for comparative purposes. The representative commodities selected for this evaluation were pepper and tomato. Furthermore, possible oxidative degradation during the sample milling step was also evaluated and avoided by the application of crio-milling conditions and ascorbic acid addition. By the proposed procedure, captan and folpet were recovered in both matrices at the 84%-105% range and with an RSD below 8% at two concentration levels 10 and 50 μg/kg. On the c