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article · Separation Science and Technology

Salting-out-assisted liquid–liquid extraction for the preconcentration and quantitative determination of eight herbicide residues simultaneously in different water samples with high-performance liquid chromatography

201725 citationsDebre Berhan University

In plain language

An analytical method combining salting-out-assisted liquid-liquid extraction with high-performance liquid chromatography has been developed to simultaneously extract and concentrate eight herbicide compounds from water. The target substances include five s-triazine herbicides and three major degradation products of atrazine. Optimised conditions achieved detection limits between 0.02 and 0.19 nanograms per millilitre and quantification limits between 0.06 and 0.65 nanograms per millilitre across the compounds. Evaluation of precision demonstrated intra-day relative standard deviations of 0.3 to 8.5 percent and inter-day values of 5.4 to 9.8 percent. The procedure was tested on spiked environmental samples, yielding relative recoveries of 72.5 to 114.6 percent for river water, 74.6 to 109.2 percent for lake water, and 62.5 to 109.6 percent for underground water.

Key takeaways

  • A method combining salting-out-assisted liquid-liquid extraction with high-performance liquid chromatography extracts five s-triazine herbicides and three atrazine metabolites simultaneously.
  • The method achieves limits of detection from 0.02 to 0.19 nanograms per millilitre and limits of quantification from 0.06 to 0.65 nanograms per millilitre.
  • Intra-day precision ranges from 0.3 to 8.5 percent, while inter-day precision ranges from 5.4 to 9.8 percent.
  • Relative recoveries in spiked river, lake, and underground water samples range from 62.5 to 114.6 percent.

Why it matters

Herbicides and their breakdown products can wash into aquatic environments, posing risks to ecosystems and drinking water supplies. This extraction and measurement technique enables the simultaneous detection of trace concentrations of multiple herbicide contaminants in diverse natural water sources, including rivers, lakes, and underground reserves.

Commercialisation angle

This technique provides an applied analytical protocol for environmental monitoring laboratories, municipal water testing facilities, and regulatory agencies monitoring pesticide contamination. Because the method has been validated on spiked river, lake, and underground water samples using standard high-performance liquid chromatography equipment, it appears ready for direct adoption and routine implementation by analytical testing services.

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Abstract

Salting˗out-assisted liquid–liquid extraction coupled with high-performance liquid chromatography was developed for selective extraction and preconcentration of five s-triazine herbicides and three major metabolites of atrazine simultaneously. Under the optimum conditions, detection and quantification limits (ng mL−1) were found in the range 0.02–0.19 and 0.06–0.65, respectively. Linearity ranges (ng mL−1) of 1–60 (ametrin), 2–160 (desethylatrazine, desisopropyl atrazine, secbumetone and terbutryn) and 4–240 (hydroxyatrazine and aziprotryn) were obtained. The relative standard deviations for the intra- and inter-day precisions were in the ranges 0.3–8.5% and 5.4–9.8%, respectively. Relative recoveries of three spiked water samples were in the ranges of 72.5–114.6, 74.6–109.2 and 62.5–109.6% for the river, lake and underground water samples, respectively.

Research topics

  • Analytical chemistry methods development
  • Analytical Chemistry and Chromatography
  • Pesticide Residue Analysis and Safety

Sustainable Development Goals

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DOI: 10.1080/01496395.2016.1276596

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