Phytochemistry (extraction, identification and measurement of active components)
Marzieh Babashpour-Asl; Marzieh Piryaei
Abstract
Background and objectives: Malus domestica Borkh. ‘Red delicious’ is one of the most economically significant fruit crops cultivated worldwide, including in Iran, with its aroma arising from a complex mixture of volatile compounds that define its sensory profile and ...
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Background and objectives: Malus domestica Borkh. ‘Red delicious’ is one of the most economically significant fruit crops cultivated worldwide, including in Iran, with its aroma arising from a complex mixture of volatile compounds that define its sensory profile and vary across species and cultivars. Deep eutectic solvents (DESs) represent an innovative class of solvents distinguished by their non-flammability, negligible volatility, low vapor pressure, thermal stability, biodegradability, minimal toxicity, and reusability, excelling in extracting bioactive compounds while preserving their structural and functional integrity while also serving dual roles as reaction media and catalysts in organic synthesis to enhance bioavailability. Headspace single-drop microextraction (HS-SDME) is a highly efficient technique for analyzing volatile and semi-volatile compounds, eliminating matrix interference with minimal solvent use, making it ideal for essential oil extraction.Methodology: This study developed an HS-SDME method for extracting apple essential oils using newly designed DESs, followed by GC/MS analysis, with key parameters, including DES composition, drop volume, sample weight, extraction temperature, and time, systematically optimized, evaluating three DESs composed of choline chloride paired with ethylene glycol, phenol, or 4-chlorophenol as hydrogen bond donors, and comparing the results with conventional hydrodistillation (HD) using a Clevenger apparatus.Results: Among the tested solvents, the combination of choline chloride and 4-chlorophenol demonstrated the highest extraction efficiency for the target analytes. Several experimental parameters influencing the efficiency of essential oil extraction using the DESs-HS-SDME method were optimized as follows: a eutectic solvent volume of 3 mL, an extraction time of 50 minutes, an extraction temperature of 80 °C, and a sample weight of 3 g. Using the DESs-HS-SDME method, 22 compounds were isolated from apple essential oil, consistent with the results obtained from the HD method. Of these compounds, 76% were monoterpenes, including α-thujene, α-pinene, camphene, sabinene, β-pinene, myrcene, α-phellandrene, p-cymene, β-phellandrene, Z-β-ocimene, E-β-ocimene, γ-terpinene, terpinolene, α-pinene oxide, trans-sabinene hydrate, cis-verbenol, neo-3-thujanol, carvacrol ethyl ether, and terpinen-4-ol acetate. Additionally, 20% were sesquiterpenes, comprising bicyclogermacrene, (E,E)-α-farnesene, germacrene B, spathulenol, and epi-cedrol. Notably, α-phellandrene, α-pinene, β-pinene, sabinene, and p-cymene were the most predominant compounds in both analytical methods employed.Conclusion: In this study, an analytical procedure was proposed for the first time for extracting essential oil from apple fruit using headspace single-drop microextraction (HS-SDME) with deep eutectic solvents (DESs). Unlike previous studies, which employed conventional solvents for HS-SDME, this work introduces DESs as a greener and more effective alternative. The DESs-HS-SDME method provides an environmentally friendly, simple, and efficient approach for essential oil extraction from apple fruit. Given their low toxicity, biodegradability, and tunable properties, DESs show great promise as suitable extraction media for isolating volatile compounds from natural samples using HS-SDME.
M. Babashpour-Asl; M. Piryaei; I. Farhang
Abstract
The genus Artemisia comprises a large number of species, some of which are cultivated commercially in a variety of applications. The high accumulation of essential oils and other terpenoids in certain members of family Asteraceae, such as wormwood (Artemisia absinthium L.), has made them useful as flavorings. ...
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The genus Artemisia comprises a large number of species, some of which are cultivated commercially in a variety of applications. The high accumulation of essential oils and other terpenoids in certain members of family Asteraceae, such as wormwood (Artemisia absinthium L.), has made them useful as flavorings. Terpenoids and phenolic compounds are also responsible for the medicinal and medical values of many members of this family. The solid-phase microextraction (SPME) is a fast, easy, efficient, highly solvent-free, and easy-to-automate method. In the present study, headspace SPME (HS-SPME) using nanostructured layered double hydroxide coated fiber in combination with gas chromatography-mass spectrometry was utilized as a monitoring technique for the collection and detection of essential oil constituents of wormwood. Experimental parameters including temperature and desorption time, temperature and extraction time, sample weight, and water content effect were tested and optimized. A temperature of 260 °C was found to be appropriate for efficient desorption. The best desorption time was obtained 2 min for all measurements. The optimized quantities were found for extraction temperature 75 °C, extraction time 25 min, sample weight 2.5 g. The added water deactivated the fiber surface by blocking the active sites; therefore, the proposed fiber is suitable for dry samples. The proposed method is simple and costly compared to conventional methods of analysis. In addition, in this method, the analysis time is shorter and could be used for the analysis of volatile compounds in medicinal plants.
