Development and validation of a multiresidue method for the analysis of 151 pesticide residues in strawberry by gas chromatography coupled to a triple quadrupole mass analyzer

Abstract

A new method was developed and validated for the simultaneous determination of 151 pesticide residues in strawberry by gas chromatography coupled to a triple quadrupole mass analyzer (GC/QqQ-MS/MS), mainly using the selected reaction monitoring (SRM) mode. The list of target compounds included various classes of pesticides such as organochlorine (OCPs), organophosphorus (OPPs), carbamates, pyrethroids, triazoles and dicarboximides. A single extraction of 10 g of sample with acetonitrile followed by liquid-liquid partition formed by the addition of 4 g of MgSO4 and 1 g of NaCl was applied in sample preparation. Cleanup of the extracts was carried out by applying dispersive solid-phase extraction (D-SPE) with primary secondary amine (PSA). The analysis time was 21 min. The method was subjected to a thorough validation procedure. The recovery data were obtained by spiking blank samples at two concentration levels (11.5 and 50 microg/kg), yielding recoveries in the range 70-110%. Precision values expressed as relative standard deviation (RSD) were lower than 18% and 22% for the intraday and interday precision, respectively. Linearity was studied in the range 10-200 microg/kg and determination coefficients (R(2)) were higher than 0.98% for all compounds. Limits of detection (LODs) and limits of quantification (LOQs) were established as 4 and 10 microg/kg, respectively. The overall uncertainty of the method was estimated at two different concentrations (11.5 and 50 microg/kg), being lower than 25% in both cases. According to the validation data and performance characteristics as well as the high sample throughput and low cost, the proposed method is suitable for routine application.