Determination of 2,4-Dichlorophenoxyacetic Acid in Water and Edible Seeds Samples Using Salt-Assisted Liquid-Liquid Extr
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Determination of 2,4-Dichlorophenoxyacetic Acid in Water and Edible Seeds Samples Using Salt-Assisted Liquid-Liquid Extraction Coupled with High-Performance Liquid Chromatography Rouhollah Heydari 1
&
Rezvan Feyzianpour 2
Received: 13 April 2020 / Accepted: 21 October 2020 # Springer Science+Business Media, LLC, part of Springer Nature 2020
Abstract A simple, fast, and effective salt-assisted liquid-liquid extraction (SALLE) technique coupled with high-performance liquid chromatography (HPLC) was developed for determination of 2,4-dichlorophenoxyacetic acid (2,4-D) in water and edible seeds samples. Due to the polar nature of the 2,4-D molecules, LC analysis was performed on a CN stationary phase by using acetonitrile and acidic water as mobile phase. Extraction was achieved based on salting-out phenomenon. Affecting variables on the extraction efficiency of the 2,4-D, such as the solvent type and its volume, type of salt and its concentration, vortex time, and sample pH, have been investigated and optimized. The target analyte was successfully extracted by acetonitrile and sodium chloride as extracting solvent and salting-out agent, respectively. Under the optimized experimental conditions, calibration curve shows good linearity (r2 > 0.9957) and precision (RSD < 6.5%) in the concentration ranges of 1.0–10,000 ng/mL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.3 and 1.0 ng/mL, respectively. The recoveries were in the range of 82.0–95.0 % with RSD values less than 7.2%. The method was successfully applied for the extraction and determination of 2,4-D in several edible seeds and water samples. Keywords 2,4-Dichlorophenoxyacetic acid . Salt-assisted liquid-liquid extraction . Edible seed . Water . HPLC
Introduction 2,4-Dichlorophenoxyacetic acid (2,4-D), a chlorinated phenoxy compound, is a systemic herbicide commonly used in rice, corn, wheat, barley, and sorghum fields to control broad-leaf weeds (Boivin et al. 2005). Studies show that the 2,4-D can lead to serious damage to humans and animals such as cancer risks, neurologic disease, reproductive risks, and immunotoxicity (Jia et al. 2017; Jervais et al. 2008). The maximum contaminant levels (MCL) of the 2,4-D for finished drinking water according to guidelines of the United State Environmental Protection Agency (US EPA) and the World Health Organization (WHO) are 0.07 and 0.03 mg/L, respectively (WHO 2011; U.S. EPA 2009). Unlike the 2,4-D amine
* Rouhollah Heydari [email protected] 1
Research Center for Environmental Determinants of Health, Health Institute, Kermanshah University of Medical Sciences, Kermanshah, Iran
2
Department of Chemistry, Payame Noor University, Tehran, Iran
salts and esters, the acid form of 2,4-D is very resistant to abiotic hydrolysis (Reregistration Eligibility Decision (RED) 2005). According to reasons above mentioned about the high toxicity, the wide applications in agriculture and resistance of the 2,4-D against biodegradation, method development for determination of this herbicide in waste
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