Evaluation of calibration approaches for quantification of pesticide residues in surface water by SPE with small-size cartridges followed by fast GC-MS

Analytical Methods Pub Date: 2013-05-13 DOI: 10.1039/C3AY40412A

Abstract

A fast GC-MS method for analysis of twenty four GC amenable pesticides in surface water was developed and validated. Extraction of pesticides using solid phase extraction (SPE) with small-size cartridges was performed. Four calibration approaches for quantification purposes, (1) acetonitrile (MeCN) standards, (2) MeCN standards with analyte protectants (APs), (3) matrix-matched standards, and (4) matrix-matched standards with APs, were investigated and statistically compared in terms of validation parameters. Linearity was studied in the concentration range of 0.01–2.5 μg L?1 with coefficients of determination (R2) higher than 0.9466. Satisfactory recoveries at three studied concentration levels (0.05, 0.1 and 1 μg L?1) in the range of 65.6–100.3% with relative standard deviation <19% were obtained. The limits of detection (LODs) and limits of quantification (LOQs) were evaluated for all approaches. LODs ranged from 0.06 to 20 ng L?1 and LOQs from 0.2 to 65 ng L?1. The developed and validated method was applied for the analysis of Danube River water samples.

Graphical abstract: Evaluation of calibration approaches for quantification of pesticide residues in surface water by SPE with small-size cartridges followed by fast GC-MS
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