Development of a Green Alternative Vortex-Assisted Dispersive Liquid–Liquid Microextraction Based on Natural Hydrophobic Deep Eutectic Solvents for the Analysis of Phthalate Esters in Soft Drinks
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High Resolution Image Download MS PowerPoint Slide A new green alternative vortex-assisted dispersive liquid–liquid microextraction method based on a natural hydrophobic deep eutectic solvent was developed for the extraction of 14 phthalic acid esters and one adipate in cold infusions and tonic waters. Analyses were carried out using ultra-performance liquid chromatography coupled to tandem mass spectrometry. Different eutectic mixtures based on the monoterpene thymol (essential oil of thyme) and medium-chain fatty acids (octanoic and decanoic acids) at different molar ratios were tested in this regard. The effect of different factors affecting extraction efficiency was optimized through a systematic approach. The method was validated by means of precision, matrix-matched calibration, recovery, and repeatability studies using two different deuterated surrogate standards (dibutyl phthalate-3,4,5,6- d 4 and dihexyl phthalate-3,4,5,6- d 4 ). The method proved to be linear (determination coefficients were higher than 0.9912) with normalized recoveries in the range between 71 and 124% (except for di- n -octyl phthalate at a low concentration level in tonic water [63%]). Then, the method was applied for the analysis of the selected compounds in 3 pineapple/green tea-based cold infusions and 8 tonic beverages. Finally, the greenness of the procedure was assessed using the Analytical Eco-Scale. This paper represents the first application of this natural hydrophobic deep eutectic solvent for the analysis of phthalate esters, and, also the first time, these compounds are analyzed in cold infusion and tonic water.
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DLLME-based methods are still widely adopted due to fast extraction kinetics, reduced solvent usage, simple sample handling, and high preconcentration capability.
“Among these, DLLME-based methods are still widely adopted due to their fast extraction kinetics, reduced solvent usage, simple sample handling, and high preconcentration capability [46,47,57,63,66,67,71,81,83,85,87,89,90].”
From Eco-Friendly Deep Eutectic Solvent-Based Extraction Technologies: A Comprehensive Review of Principles, Applications, and Comparative Insights (2026) · cites this paper as [63]
Vortex-assisted DLLME uses mechanical agitation and offers a simple, economical, instrumentally minimal approach.
“In vortex-assisted DLLME, mechanical agitation is applied, offering a simple, economical, and instrumentally minimal approach [56,59,63,82,99].”
From Eco-Friendly Deep Eutectic Solvent-Based Extraction Technologies: A Comprehensive Review of Principles, Applications, and Comparative Insights (2026) · cites this paper as [63]
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Conde-Díaz, A., Santana‐Mayor, Á., Socas-Rodríguez, B., Herrera‐Herrera, A. V., & Rodríguez‐Delgado, M. Á. (2026) · Sustainable Chemistry and Pharmacy · doi:10.1016/j.scp.2026.102423
Self-citationPandey, A. K., Kumar, A., Bano, S., Chowdhury, S., & Roy, S. K. (2026) · Journal of Agricultural and Food Chemistry · doi:10.1021/acs.jafc.6c06077
Wang, X., Dong, H., Xie, B., Yang, C., & Zhao, T. (2026) · ACS Omega · doi:10.1021/acsomega.6c07725
- Authors
- Santana-Mayor, Á., Herrera-Herrera, A. V., Rodríguez-Ramos, R., Socas-Rodríguez, B., & Rodríguez-Delgado, M. Á.
- Affiliations
- Departamento de Química, Unidad Departamental de Química Analítica, Facultad de Ciencias, Universidad de La Laguna (ULL), Avenida Astrofísico Francisco Sánchez, s/no, 38200 San Cristóbal de La Laguna (Tenerife), España
- Instituto Universitario de Bio-Orgánica Antonio González, Universidad de La Laguna (ULL), Avda. Astrofísico Fco. Sánchez, 2, 38200 San Cristóbal de La Laguna, España
- Laboratory of Foodomics, Institute of Food Science Research, CIAL, CSIC, Nicolás Cabrera 9, 28049 Madrid, Spain
- Venue
- ACS Sustainable Chemistry & Engineering
- Publisher
- American Chemical Society (ACS)
- Published
- 2021-01-20
- Volume
- 9
- Issue
- 5
- Pages
- 2161-2170
- ISSN
- 2168-0485 (ISSN-L)
- OpenAlex
- W3124148799
- Cited by
- 59
- References
- 40
- Citations by year
- 2026: 5 · 2025: 9 · 2024: 14 · 2023: 14 · 2022: 12 · 2021: 5
- FWCI
- 5.64
- Type
- journal article
- Language
- en
- Open access
- hybrid
- doi.org
- Locations
- ACS Sustainable Chemistry & Engineering (publishedVersion, cc-by)
- DIGITAL.CSIC (Spanish National Research Council (CSIC)) (submittedVersion)
- Funders
- Ministerio de Econom?a, Industria y Competitividad, Gobierno de Espa?a (AGL2017-89257-P)
- Topics
- Physical Sciences › Chemistry › Analytical Chemistry › Analytical chemistry methods development
- Physical Sciences › Chemical Engineering › Catalysis › Ionic liquids properties and applications
- Physical Sciences › Chemistry › Spectroscopy › Analytical Chemistry and Chromatography
- Keywords
- phthalates, adipate, deep eutectic solvents, hydrophobic deep eutectic solvents, vortex-assisted dispersive liquid-liquid microextraction, green analytical chemistry, thymol, medium-chain fatty acids, octanoic acid, capric acid, cold infusion, tonic water, soft drinks, Analytical Eco-Scale, UPLC-MS/MS
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