A Sustainable Supramolecular Deep Eutectic Solvent System for Dispersive Liquid–Liquid Microextraction Followed by HPLC for the Determination of Melamine in Milk Samples
Open accessAbstract
This work presents the development and application of an innovative green supramolecular deep eutectic solvent (SUPRADES)-based DLLME approach for the extraction and quantification of melamine in milk matrices. For this purpose, thymol and nonanoic acid were combined to create a hydrophobic DES, which was then utilized as the extraction solvent. Additionally, a ternary SUPRADES based on a hydrophilic DES composed of choline chloride and ethylene glycol and doped with β-cyclodextrin (β-CD) was prepared and applied as the disperser solvent. Critical parameters were optimized systematically, yielding the following optimal conditions: Extraction sol v ent volume: 150 μL; disperser solvent: 600 μL; β-CD: 1% ( w / v ); pH: 7; extraction time: 1 min; and sample solution volume: 5 mL. Interestingly, the salting-out step did not affect the extraction efficiency. The optimized approach showed good linearity (100–900 ng/mL) with R 2 = 0.998 when validated with matrix-matched calibration standards. The LOD and LOQ were 27 and 81 ng/mL, respectively, and the enrichment factor was 41. Method accuracy and precision were evaluated through recovery studies using milk samples fortified with melamine at three concentration levels (200, 500, and 800 ng/mL), and the recovery values were obtained in the range of 92–107%, with RSD < 5%. A greenness score of 79 was attained by the method, as quantified by the advanced ComplexMoGAPI. Lastly, this technique was successfully applied to extract and determine melamine in real samples of powdered milk, infant formula, and raw milk with acceptable and satisfactory results.
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In situ DES generation streamlines the extraction procedure by forming the solvent directly within the sample matrix, which reduces reagent usage, minimizes solvent preparation requirements, and enhances overall sustainability.
“In situ DES generation streamlines the extraction procedure by forming the solvent directly within the sample matrix, which reduces reagent usage, minimizes solvent preparation requirements, and enhances the overall sustainability of the process [54,100].”
From Eco-Friendly Deep Eutectic Solvent-Based Extraction Technologies: A Comprehensive Review of Principles, Applications, and Comparative Insights (2026) · cites this paper as [100]
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- Authors
- Sadek, M., Sarkis, N., & Jangi, G.
- Affiliations
- University of Aleppo (SY)
- Corresponding author
- Sadek, Modar
- Venue
- Results in Chemistry
- Publisher
- Elsevier BV
- Published
- 2026-02
- Volume
- 20
- Pages
- 103057
- ISSN
- 2211-7156 (ISSN-L)
- OpenAlex
- W7119794506
- Cited by
- 5
- References
- 45
- Citations by year
- 2026: 5
- FWCI
- 13.04
- Type
- journal article
- Language
- en
- Open access
- gold
- doi.org
- Licence
- Locations
- Results in Chemistry (publishedVersion, cc-by-nc-nd)
- DOAJ (DOAJ: Directory of Open Access Journals) (submittedVersion, cc-by-sa)
- Topics
- Physical Sciences › Chemistry › Analytical Chemistry › Analytical chemistry methods development
- Physical Sciences › Chemical Engineering › Catalysis › Ionic liquids properties and applications
- Life Sciences › Agricultural and Biological Sciences › Food Science › Melamine detection and toxicity
- Keywords
- melamine, milk, deep eutectic solvents, dispersive liquid-liquid microextraction, green analytical chemistry, β-cyclodextrin, choline chloride, thymol, nonanoic acid, salting-out, infant formula, raw milk, milk powder, food contaminant analysis
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