Revisiting quick, easy, cheap, effective, rugged, and safe parameters for sample preparation in pesticide residue analysis of lettuce by liquid chromatography-tandem mass spectrometry.

A new analytical method using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) procedure for multi-residue determination of 16 multiclass pesticides in five different types of lettuce was developed using high-performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry. The QuEChERS procedure was optimized in terms of extractor solvent, partitioning salts and clean-up salts, through recovery, gravimetric analysis and matrix-effect studies. Microwave extraction and the use of disposable pipette extraction in the clean-up step were also tested, providing interesting alternatives to the traditional QuEChERS method, depending on the pesticides properties. The use of a laboratory-made phenyl-type sorbent, based on silica and poly(2-phenylpropyl)methylsiloxane, was studied in the clean-up step, presenting promising results as a substitute for primary secondary amine (PSA). The optimized QuEChERS method was defined employing acetonitrile, citrate buffer and clean-up with PSA, MgSO4 and graphitized carbon black. The method developed was validated according to Document SANTE/11945/2015 and proved to be selective, accurate and precise, obtaining limits of quantification from 5μgkg-1 and recoveries in the range of 70-120% with relative standard deviation≤20%. The method was applied on 14 real samples from commercial markets in Brazil and 21% of the samples analyzed presented irregularities, according to local pesticides regulations.