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.

Development of a Multi-mycotoxin Analysis in Beer-based Drinks by a Modified QuEChERS Method and Ultra-High-Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

“…In order to develop a simple clean-up of mycotoxins, the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method, 20 which has recently attracted attention as a simple clean-up method for multiple pesticide residues analysis, [21][22][23] was examined in beer-based drinks (beer, low-malt beer, new genre, and nonalcoholic). The characteristic features of the QuEChERS method are as follows: (1) extraction with acetonitrile in a disposable tube, followed by the salting out and removal of water from acetonitrile using sodium chloride (NaCl) and anhydrous magnesium sulfate (MgSO4); (2) purification with dispersive solid phase extraction (dSPE), in which the extract is processed by shaking with either a primary-secondary amine (PSA) silica gel alone, or PSA plus C18 or graphite carbon black (GCB).…”

Simultaneous determination of 103 pesticide residues in tea samples by LC‐MS/MS

“…Generally speaking, the determination of routine pesticide multi-residues in tea, water or other food samples is usually carried out by GC in combination with electron capture detection [2,3], flame photometric detection [4], MS [5 -7] and MS/MS [8,9]. These methods are suitable for analysis of thermally stable, low-polar and volatile pesticides.…”

Multiresidue method for the analysis of more than 140 pesticide residues in fruits and vegetables by gas chromatography coupled to triple quadrupole mass spectrometry

“…The sample was centrifuged at 4000 rpm (2750g) for 6 min in a highvolume centrifuge. An aliquot of the upper layer (1 ml) was placed in a 2.0-ml Eppendorf safe-lock micro test tube containing 25 mg of PSA and 150 mg of anhydrous MgSO 4 . The tubes were sealed and carefully shaken with a minishaker before being centrifuged at 6000 rpm (3500g).…”

“…22 -25 Their main advantages include high recoveries obtained for a wide range of pesticide polarities, adequate trueness and precision, high sample throughput, simple instrumentation and materials, and low cost per sample. This method is based on an acetonitrile extraction and an induced partition by addition of MgSO 4 and NaCl. Then, a dispersive solid-phase extraction (D-SPE) with primary secondary amine (PSA) is applied as clean up.…”