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

• Published in: Rapid communications in mass spectrometry 2007-07, Vol.21 (14), p.2282-2294
• Main Authors: Bolaños, Patricia Plaza, Moreno, José Luis Fernández, Shtereva, Deyana D., Frenich, Antonia Garrido, Vidal, José Luis Martínez
• Format: Article
• Language: English
• Subjects: Algorithms; Complex Mixtures - analysis; Food Analysis - methods; Food Contamination - analysis; Fragaria - chemistry; Fruit - chemistry; Gas Chromatography-Mass Spectrometry - methods; Pesticides - analysis; Reproducibility of Results; Sensitivity and Specificity; Specimen Handling - methods; Spectrometry, Mass, Electrospray Ionization - methods
• ISSN: 0951-4198; 1097-0231
• DOI: 10.1002/rcm.3091

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 µg/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 µg/kg and determination coefficients (R2) were higher than 0.98% for all compounds. Limits of detection (LODs) and limits of quantification (LOQs) were established as 4 and 10 µg/kg, respectively. The overall uncertainty of the method was estimated at two different concentrations (11.5 and 50 µg/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. Copyright © 2007 John Wiley & Sons, Ltd.