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 in the exposure monitoring in occupational health.

Highlights

  • Pesticides are widely used for agricultural purposes around the world

  • Butachlor is structurally belonging to the chloroacetanilide family, and chlorpyrifos is in the organophosphorus pesticide category

  • Since the best response for butachlor obtained in the temperature 80 ̊C, for improving the simultaneous extraction of butachlor and chlorpyrifos, temperature of 80 ̊C was chosen as the optimum temperature

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Summary

Introduction

Pesticides are widely used for agricultural purposes around the world. Application of pesticides in agriculture has increased productivity and has led to the increase yields in farming. Among the various pesticides available; butachlor and chlorpyrifos are the ones most widely used in developing countries, including Iran by the relevant plant protection organization. Solid-phase extraction (SPE) [11]-[17], supercritical fluid extraction (SFE) [18], and matrix solid-phase dispersion (MSPD) [19] is the other more selective approach in this field. These methods are multistage, expensive, laborious, and consume long time as well as; in these methods, a large amount of organic solvents are applied to extract the analysts of interest [20]

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