Journal Article

Influence of QuEChERS modifications on recovery and matrix effect during the multi-residue pesticide analysis in soil by GC/MS/MS and GC/ECD/NPD

Łozowicka, Bożena, Rutkowska, Ewa, Jankowska, Magdalena

2017

Overview

A QuEChERS extraction followed by GC/MS/MS and GC-μECD/NPD for 216 pesticide and metabolites determination in soil simultaneously were developed and compared. Volume of water, volume and polarity of solvent, and cleanup sorbents (C18, GCB, PSA) were optimized. The QuEChERS with and without purification step were applied to estimate effectiveness of the method. The recovery and matrix effect (ME) were critical parameters within each tested procedure. The optimal method without cleanup was validated. Accuracy (expressed as recovery), precision (expressed as RSD), linearity, LOQ, and uncertainty were determined. The recoveries at the three spiking levels using matrix-matched standards ranged between 65 and 116% with RSD ≤17 and 60–112% with RSD ≤18% for MS/MS and μEC/NP, respectively. The LOQ ranged from 0.005–0.01 mg/kg for MS/MS to 0.05 mg/kg for μEC/NP. The ME for most of pesticides resulted in enhancement of the signal and depended on the analyte and detection system: MS/MS showed ME from −25 to 74%, while μEC/NP from −45 to 96%. A principal component analysis was performed to explain the relationships between physicochemical parameters and ME of 216 pesticides. The QuEChERS protocol without the cleanup step is a promising option to make the method less expensive and faster. This methodology was applied in routine analysis of 263 soil samples in which p,p’ DDT was the most frequently detected (23.5% of samples) and pendimethalin with the highest concentration (1.63 mg/kg).

• Publisher: Springer Berlin Heidelberg,Springer Nature B.V
• Subject: Agrochemicals / Aquatic Pollution / Atmospheric Protection/Air Quality Control/Air Pollution / DDT / DDT (pesticide) / Earth and Environmental Science / Ecotoxicology / Environment / Environmental Chemistry / Environmental cleanup / Environmental Health / Environmental science / gas chromatography-mass spectrometry / Gas Chromatography-Mass Spectrometry - methods / Limit of Detection / Linear Models / Linearity / Metabolites / Pendimethalin / Pesticide residues / Pesticide Residues - analysis / Pesticide Residues - chemistry / Pesticide Residues - isolation & purification / Pesticides / Physicochemical properties / Polarity / principal component analysis / Principal components analysis / Purification / Recovery / Reproducibility of Results / Research Article / soil / Soil analysis / Soil Pollutants - analysis / Soil Pollutants - chemistry / Soil Pollutants - isolation & purification / soil sampling / Soils / solvents / Sorbents / Tandem Mass Spectrometry - methods / uncertainty / Waste Water Technology / Water Management / Water Pollution Control