Optimization of Solid Phase Microextraction Procedure Followed by Gas Chromatography with Electron Capture Detector for Pesticides Butachlor and Chlorpyrifos

Abstract

In this study, headspace solid phase microextraction (HS-SPME) followed by gas chromatography using electron capture detection system (GC-ECD) were developed for the determination of chloraacetanilide (butachlor) and chlorpyrifos presented in biological samples. Different parameters affecting the extraction procedure were optimized including extraction time (30 minutes), extraction temperature (80˚C), sample volume (3 mL), sample pH (2), added NaCl (0.3 gram) and sample stirring rate (400 rpm). Different concentrations of 1 -100 ng/ml were applied for butachlor and a linear calibration curve was obtained. Furthermore, a similar linearity was obtained for chlorpyrifos, using a concentration range of 1 -250 ng/ml. The limit of detection (LOD) obtained for butachlor and chlorpyrifos were 0.088 and 0.53 ng/ml respectively. The optimized methods for both compounds were validated using two concentrations of 25 and 50 ng/ml in spiked urine samples. Obtained recoveries of spiked urine samples were 83.06% -99.8% with RSD of lower than 11%. Optimized technique was simple, inexpensive, solvent free and fast in comparison with other conventional methods and had compatibility with the chromatographic analytical system. This method offers low detection limits to analyze pesticides in urine samples that are very important * Corresponding author. F. Ghavidel et al. 536in the exposure monitoring in occupational health.

Application of solid‐phase extraction: High‐resolution mass spectrometry analysis strategy in the characterization and quantification of amide herbicides in aquatic products

“…Current methods used to monitor herbicide residues include LC with ultraviolet [9,10] or MS/MS detectors [11][12][13], and GC with flame ionization [14], electron capture [15,16], or MS detectors [17][18][19]. LC-MS is widely used and the triple quadrupole MS has become a routine detection tool for the analysis of multiresidue pesticides and veterinary drug residues.…”

Synthesis of molecularly imprinted nanoparticles for selective exposure assessment of permethrin: optimization by response surface methodology

“…The drawbacks of traditional sample preparation techniques have actuated a growing tendency towards new, inexpensive, and quite fast approaches. In this regard, several novel techniques such as solid phase extraction (SPE) [33,34], solid-phase microextraction (SPME) [35,36], matrix solidphase dispersion (MSPD) [37,38], stir bar sorption extraction (SBSE) [39,40], supercritical fluid extraction (SFE) [41], accelerated solvent extraction (ASE) [42,43] and liquid-phase microextraction (LPME) [44,45] have been developed in order to improve organic material extraction throughput in terms of time, solvent consumption, reproducibility and enrichment factor (EF). Despite the benefits of these methods, all of them suffer from lack of selectivity limiting their application in large-scale analyses.…”