Deep eutectic solvent–based headspace single-drop microextraction for the quantification of terpenes in spices
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Deep eutectic solvents (DESs) were investigated as extracting solvent for headspace single-drop microextraction (HS-SDME). The extraction efficiency of 10 DESs mainly composed of tetrabutylammonium bromide (N 4444 Br) and long-chain alcohols was evaluated for the extraction of terpenes from six spices (cinnamon, cumin, fennel, clove, thyme, and nutmeg). The DES composed of N 4444 Br and dodecanol at a molar ratio of 1:2 showed the highest extraction efficiency and was selected to conduct the extractions of terpenes in the rest of the study. HS-SDME was optimized by design of experiments. Only two parameters from the four studied showed a significant influence on the efficiency of the method: the extraction time and the extraction temperature. The optimal extraction conditions were determined by response surface methodology. All extracts were analyzed by gas chromatography coupled to mass spectrometry (GC-MS). More than 40 terpenes were extracted and identified in nutmeg, the richest extract in terpenes in this study. Quantitative analysis based on 29 standards was conducted for each extract. Good linearity was obtained for all standards (R 2 > 0.99) in the interval of 1 to 500 μg/g. Limits of quantification ranged from 0.47 μg/g (borneol) to 86.40 μg/g (α-farnesene) with more than half of the values under 2 μg/g. HS-SDME is simple, rapid, and cheap compared with conventional extraction methods. The use of DESs makes this extraction method "greener" and it was shown that DESs can be suitable solvents for the extraction of bioactive compounds from plants.
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Triaux et al.'s DES-HS-SDME application to 27 terpenes showed that half of the studied compounds had LOQs lower than 2 μg/g.
“The application to 27 different terpens showed that half of the studied compounds had LOQs lower than 2 μg/g”
From Microextraction Techniques with Deep Eutectic Solvents (2020) · cites this paper as [96]
Section 3.3 (Calibration) reports that more than half of the studied compounds had LOQs below 2 µg/g, but it gives the calibration count as 29 terpenes, not 27. Section 3.1 uses 27 for a separate solvent-screening comparison, not for the LOQ result. (LLM, conf=0.91)
Experimental — accuracy not yet measuredDES-HS-SDME is a simple, cheap, green, and efficient technique for the extraction of terpenes.
“Therefore, DES-HS-SDME is a simple, cheap, green, and efficient technique for the extraction of terpenes [96].”
From Microextraction Techniques with Deep Eutectic Solvents (2020) · cites this paper as [96]
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- Authors
- Triaux, Z., Petitjean, H., Marchioni, E., Boltoeva, M., & Marcic, C.
- Affiliations
- Centre National de la Recherche Scientifique (FR)
- Corresponding author
- Marcic, Christophe
- Venue
- Analytical and Bioanalytical Chemistry
- Published
- 2020-01-11
- Volume
- 412
- Issue
- 4
- Pages
- 933-948
- ISSN
- 1618-2642 (ISSN-L)
- 1618-2650
- OpenAlex
- W3000579260
- Cited by
- 77
- References
- 45
- Citations by year
- 2026: 8 · 2025: 9 · 2024: 11 · 2023: 19 · 2022: 12 · 2021: 13 · 2020: 5
- FWCI
- 6.35
- Type
- journal article
- Language
- en
- Open access
- green
- hal.science
- Licence
- Locations
- Analytical and Bioanalytical Chemistry (publishedVersion)
- PubMed (publishedVersion)
- HAL (submittedVersion, other-oa)
- Funders
- Association Nationale de la Recherche et de la Technologie (CIFRE Contract n°2016/0447)
- 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
- deep eutectic solvents, headspace single-drop microextraction, terpenes, spices, tetrabutylammonium bromide, dodecanol, green extraction, nutmeg, cinnamon, cumin, fennel, Syzygium aromaticum, thyme, borneol, α-farnesene, extraction optimization
- MeSH terms
- Cinnamomum zeylanicum, Gas Chromatography-Mass Spectrometry, Plant Extracts, Solvents, Terpenes, Spices, Myristica, Syzygium, Cuminum, Foeniculum, Thymus Plant, Liquid Phase Microextraction
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