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DOE OSTI · 1833548

Comparing the extraction performance of cyclodextrin-containing supramolecular deep eutectic solvents versus conventional deep eutectic solvents by headspace single drop microextraction

Farooq, Muhammad Qamar·Zeger, Victoria R.·Anderson, Jared L.
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Abstract

A headspace single drop microextraction (HS-SDME) method coupled with high performance liquid chromatography was developed to compare the extraction of eighteen aromatic organic pollutants from aqueous solutions using cyclodextrin-based supramolecular deep eutectic solvents (SUPRADESs) and alkylammonium halide-based conventional deep eutectic solvents (DESs). Different derivatives of beta-cyclodextrin (β-CD) were employed as hydrogen bond acceptors (HBA) in SUPRADESs and the extraction performance investigated. SUPRADES comprised of the 20 wt% native β-CD HBA provided the highest enrichment factors of analytes compared to SUPRADESs comprised of other derivatives of β-CD (random methylated β-cyclodextrin, heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin, and 2-hydroxypropyl β-cyclodextrin). In addition, native β-CD and its derivatives were dissolved in the neat DESs and their effect on the extraction of analytes examined. Dissolution of 20 wt% native β-CD in the choline chloride ([Ch + ][Cl - ]):2Urea DES resulted in a significant increase in the extraction efficiencies of target analytes compared to the neat [Ch + ][Cl - ]:2Urea DES. Under optimum conditions, the extraction method required a solvent microdroplet of 6.5 μL, 1000 rpm stir rate, 30% (w/v) salt concentration, and a temperature of 40 °C. The tetrabutylammonium chloride: 2 lactic acid DES resulted in the highest enrichment factors while the [Ch + ][Cl - ]:2Urea DES had the lowest for most of the analytes among the evaluated solvents. The method provided limits of detection (LODs) down to 35 μg L -1 . Finally, the developed method was applied for the analysis of spiked tap and lake water, where relative recoveries ranging from 83.7% -119.7% and relative standard deviations lower than 19.2% were achieved.

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRYcyclodextrinsheadspace single drop microextractionhigh performance liquid chromatographyorganic pollutantssupramolecular deep eutectic solvents

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Farooq, Muhammad Qamar, Zeger, Victoria R., Anderson, Jared L.. 2022-10-03. Comparing the extraction performance of cyclodextrin-containing supramolecular deep eutectic solvents versus conventional deep eutectic solvents by headspace single drop microextraction. https://doi.org/10.1016/j.chroma.2021.462588

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