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Extraction and Derivatization of Chlorophenoxy Acid Pesticides: Performing Two DLLME with One Extracting Phase

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Abstract

A novel, simple and convenient method based on dispersive liquid–liquid microextraction (DLLME) and derivatization was developed and applied for isolation of a couple of selected chlorophenoxy acid herbicides from aquatic media. In the first step, analytes were extracted from acidic media into carbon tetrachloride phase using a DLLME. In following, derivatization was carried out on extracted compounds by means of methylation with an acidic methanol solution to increase their volatility and detectability in gas chromatography analysis. Finally, the derivatized analytes were re-extracted in the carbon tetrachloride phase in the second DLLME. Some important extraction parameters such as the nature and volume of the extraction solvent, disperser solvent, pH and the ionic strength were optimized. Subsequently, the developed method was validated by gas chromatography–mass spectrometry (GC–MS). Under the optimum conditions, the linearity was studied at the concentration range of 1–100 µg L−1 with a satisfactory coefficient of determination (r 2 > 0.99) for all the studied analytes. Also, the relative standard deviations (RSD %) values were from 2.5 to 4.5 % at the concentration levels of 2 and 50 µg L−1. The detection limits were found to be in the range of 0.15–0.31 µg L−1 using time-scheduled selected ion monitoring (SIM) mode. The developed method was successfully applied to the extraction and determination of chlorophenoxy acid herbicides in the river and tap water samples.

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Acknowledgments

The Research Council of Islamic Azad University is thanked for supporting the Project.

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Correspondence to Ali Es’haghi.

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Ebrahimi, R., Feizbakhsh, A. & Es’haghi, A. Extraction and Derivatization of Chlorophenoxy Acid Pesticides: Performing Two DLLME with One Extracting Phase. Chromatographia 79, 515–520 (2016). https://doi.org/10.1007/s10337-016-3042-z

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  • DOI: https://doi.org/10.1007/s10337-016-3042-z

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