Abstract

ABSTRACTA simple and rapid dispersive liquid–liquid microextraction (DLLME) technique coupled with gas chromatography–ion trap mass spectrometry (GC–MS) was developed for the extraction and analysis of five endosulfan pesticides from the fish pond water. In this work, different parameters affecting the extraction process such as the type and volume of extraction solvent, type and volume of disperser solvent, and extraction time were studied and optimized. Under optimized conditions, the enrichment factor ranged from 189 to 269 and the relative recovery ranged from 88.5% to 94.9%. The linear range was 2.0–80.0 µg/L; the limits of detection and quantitation were in the range 0.04–1.06 µg/L and 0.12–3.53 µg/L, respectively. The relative standard deviations were in the range 0.94%–2.08% (n = 5). The obtained results show that DLLME combined with GC–MS is a fast and simple method for the determination of endosulfan pesticides in fish pond water.

Highlights

  • Endosulfan, called thiodan, is an organochlorine pesticide that is extensively used in agricultural production [1]

  • The series of solvents were compared for the extraction of the studied endosulfan pesticides, and were evaluated for extraction using the following model: 5.0 mL of sample spiked with each endosulfan pesticide at concentration of 1.0 mg/mL, 1.0 mL of dispersive solvent and 20.0 mL of extraction solvent were used

  • The results revealed that the series of ethanol and tetrachloroethylene has the highest extraction efficiency in comparison with the other series

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Summary

Introduction

Endosulfan, called thiodan, is an organochlorine pesticide that is extensively used in agricultural production [1]. The concentration of endosulfan pesticides in the water is very low in these cases Conventional extraction methods such as liquid–liquid extraction (LLE) [4] and solidphase extraction (SPE) [5] require large volumes of organic solvents and are time-consuming. A few new preconcentration technologies have been introduced, such as single-drop microextraction (SDME) [7], hollow-fibre-protected liquid-phase microextraction (HF-LPME) [8], supercritical fluid extraction (SFE) [9], and molecularly imprinted polymer-based solid-phase micro-extraction (MIP-SPME) [10] All of these techniques have their own advantages; there can be relatively expensive and long extraction times. A DLLME sample preparation method was developed for the preconcentration of five endosulfan pesticides from fish pond water. £100; where Vsed and V0 are the volumes of sedimented phase and sample solution, respectively

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