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This study aimed to compare the effects of two extraction techniques (conventional n-hexane and supercritical CO2) on the oil extraction yields, fatty acids profile, anti-hyaluronidase activity, oxidative stability, and in vitro bioactivities of oils from Sacha Inchi (Plukenetia volubilis). Higher oil extraction yield (99 %) was achieved using the SC-CO2, although similar fatty acids profiles were depicted between both treatments (p < 0.05). The SC-CO2 oil presented higher anti-hyaluronidase (31 %) activity, but lower oxidative stability (5.05 h) compared to the solvent extraction (10 %, and 5.3 h, respectively). In vitro assays further revealed that the best human normal colon cells (FHC) cell viability (100 %), anti-inflammatory (50 % lower NO production), and antioxidant (20 % ROS reduction) activities were consistently observed in both extraction treatments at concentrations of 50 µg/mL and higher. These findings highlight the potential of supercritical CO2 extraction in yielding Sacha Inchi oil with enhanced bioactive properties without the disadvantages of the use of organic solvents extraction.

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Cinnamomum tamala leaf (CTL), also known as Indian bay leaf, is used all over the world for seasoning, flavoring, and medicinal purposes. These characteristics could be explained by the presence of several essential bioactive substances and lipid derivatives. In this work, rapid screening and identification of the chemical compounds in supercritical (SC)-CO2 extracts of CTL by use of UPLC-Q-TOF-MSE with a multivariate statistical analysis approach was established in both negative and positive mode. A total of 166 metabolites, including 66 monocarboxylic fatty acids, 52 dicarboxylic fatty acids, 27 fatty acid amides, and 21 cinnamic acid derivatives, were tentatively identified based on accurate mass and the mass spectrometric fragmentation pattern, out of which 142 compounds were common in all SC-CO2 extracts of CTL. Further, PCA and cluster hierarchical analysis clearly discriminated the chemical profile of analyzed extracts and allowed the selection of SC-CO2 extract rich in fatty acids, fatty acid amides, and other bioactive constituents. The result showed that the higher number of compounds was detected in CTL4 (300 bar/55 °C) extract than the other CTL extracts. The mono- and di-carboxylic fatty acids, fatty acid amides, and cinnamic acid derivatives were identified in CTL for the first time. UPLC-Q-TOF-MSE combined with chemometric analysis is a powerful method to rapidly screen the metabolite profiling to justify the quality of CTL as a flavoring agent and in functional foods.

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To obtain oil from bee brood, which was dried using a tray drying method, this study used the supercritical CO2 extraction method. Extraction occurred at temperatures between 40-60 °C and low pressures of 180-220 bar for 1.5 h, with a high pressure of 600 bar for 1 h. The study investigated both the yield and chemical properties of the extracted bee brood oils. Supercritical CO2 extraction of tray-dried bee brood at 600 bar pressure demonstrated higher oil extraction efficiency compared to lower pressures (180-220 bar). At temperatures of 40-60 °C, total phenolic compounds increased while total flavonoids decreased. The extracted oil exhibited antioxidant activity, primarily due to quercetin. Despite decreased acid, iodine, and saponification values, peroxide value slightly increased but remained below 12 meqO2/kg of oil. The make-up of the fatty acids changed. At 600 bar, palmitic and oleic acids were the most common, while myristic, linoleic, and docosadienoic acids decreased. At 600 bar, eicosadienoic acid was absent. The defatted bee brood retained significant essential and non-essential amino acids, indicating its potential for further development as a protein source.

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In this study, recovery of phenolic substances with Soxhlet extraction, (SE) ultrasound-assisted extraction (UAS), and supercritical CO2 (SC-CO2) extraction methods from chemical sludge obtained with chemical precipitation (FeCl3/PACS, Ca(OH)2/PACS, perlite/PACS, FeCl3/cationic polyelectrolyte) of lemon processing wastewater was investigated. The effect of used coagulants/flocculants and pH on COD and total phenolic substance content (TPC) removal was researched. Recovered phenolic substance profiles were also determined with HPLC-DAD. Additionally, response surface methodology was used to determine optimum treatment conditions. ANOVA analysis showed that pH is a more important variable than coagulant/flocculant doses for all chemical precipitation experimental sets. The highest removal efficiencies for COD and TPC was obtained in FeCl3/PACS (COD: 72.0 %, TPC: 93.7 %). Optimum dose values were determined as pH: 4, FeCl3: 3000 mg/L, PACS: 400 mg/L for FeCl3/PACS, pH: 6.5, Ca(OH)2: 1500 mg/L, PACS: 300 mg/L for Ca(OH)2/PACS, pH: 5.5, PACS: 7000 mg/L, perlite: 50 g/L for perlite/PACS, pH: 4.5, FeCl3: 500 mg/L, polyelectrolyte: 4 mg/L for FeCl3/polyelectrolyte. TPC removal efficiencies were determined as 55 %, 35 %, 57 % and 58 % in these conditions, respectively. Maximum TPC in extracts was determined as 39.03 mg GAE/g extract, 8.81 mg GAE/g extract, and 4.34 mg GAE/g extract for SE, UAS, and SC-CO2, respectively. TPC recovery efficiencies (RTPC) for all chemical sludge were SE > UAS > SC-CO2. Additionally, the TPC profile has shown a difference depending on the extraction method. According to the results of this study, it was concluded that the coagulation-flocculation process may be a suitable alternative for fruit juice processing industry wastewater in terms of both reducing environmental pollution and recovering polyphenolics from formed sludge. Consequently, this study presented a different perspective on the recovery from wastes with valuable substance recovery from chemical sludge.

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Hericium erinaceus (HE), a widely utilized natural remedy and dietary source, has garnered significant attention for its therapeutic potential in various diseases. In this study, we employed supercritical fluid extraction (SFE) technology to isolate the bioactive compounds from HE's fruiting body. Comprehensive assessments of the antioxidant and antibacterial activities were conducted, along with in vitro investigations on the human colon cancer cell line (HCT-8). The SFE rate served as the evaluation metric, while the variables of extraction time, pressure, and temperature were systematically examined. By integrating the response surface center composite design, we successfully optimized the extraction process, yielding optimal parameters of 80 min, 30 MPa, and 35 °C, thus resulting in an extraction rate of 2.51%. These optimized conditions exhibited considerable antioxidant capacity, anticancer activity, and antibacterial potential. Furthermore, we employed graded alcohol extraction to refine the crude extracts, thereby confirming superior anticancer effects under a 70% alcohol precipitation. To elucidate the composition, Fourier-transform infrared spectroscopy (FT-IR) and gas chromatography-mass spectrometry (GC-MS) were employed to analyze the crude extracts and isolates of HE, facilitating a comparative analysis of six HE varieties. Our findings suggest that sterol derivatives hold promise as the active component against the colon cancer HCT-8 cell line. In conclusion, this study underscores the potential of HE SFE in the development of functional foods or alternative drugs for colon cancer treatment, thus opening new avenues for therapeutic interventions.

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Green extraction of supercritical liquid CO2 (SCFE-CO2) using co-solvent methanol can produce a more complete phenolic acid composition and a higher quantity when compared to those without using co-solvent. The extract was devoid of toxicity. SCFE-CO2 is carried out by putting 100 g of Quercus infectoria gall of size 0.3 mm into extraction tube at temperature of 60 °C and the pressure of 20 MPa with a CO2 flow rate of 25 ml/min using co-solvent methanol with variation of flow speed 0.05, 0.5, 1.5, 3, and 6 for 60 min. The extract is analyzed using LC-MS/MS, the total phenolic content is determined using the Folin-Ceocateu method, and the toxicity value is determined using the Vero cell. According to the results, the green method of extracting SCFE-CO2 with methanol co-solvent can produce a peak and identify about 27 phenolic compounds, and increasing the rate of flow of methane co-solvent will greatly affect the outcome of the extraction to a flow rate of 0.5 ml/min, while adding a co-solvent with a flow speed above 0.5 does not affect the result. Repeated extraction of some of the largest phenolic peaks provide phenol content with minimal extract variability (div. sd. 0.1%), and the addition of soluble methanol will also increase the TPC concentration but does not increase the IC50 toxicity value above 1000.

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Wild strawberry (Fragaria vesca L.) seed oil (WSO) recovered by two methods-cold pressing (CP) and extraction with supercritical carbon dioxide (SCO2E)-taking into account the different extraction times, was characterized for its composition and quality. The cytotoxicity assessment of WSOs was also carried out using the normal human dermal fibroblast (NHDF) cell line. Tocopherol and total polyphenol contents were significantly higher in WSO recovered by SCO2E, up to 1901.0 and 58.5 mg/kg, respectively, in comparison with CP oil. In CP oil, the highest content of carotenoids and squalene was determined (123.8 and 31.4 mg/kg, respectively). Phytosterol summed up to 5396 mg/kg in WSO collected in 30 min of SCO2E. Moreover, the highest oxidative stability was found for this oil. All studied WSOs were non-cytotoxic in lactate dehydrogenase (LDH) leaching and sulforhodamine B (SRB) assays; however, oils collected by SCO2E in 15 and 30 min were found to be cytotoxic in the tetrazolium salt (MTT) test, with the CC50 at a concentration of 3.4 and 5.5%, respectively. In conclusion, the composition of WSO indicates that, depending on the method of its recovery, seeds can have different bio-potencies and various applications.

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The wine industry generates large quantities of by-products each year. Therefore, this work aimed to isolate and evaluate the oil and protein fractions of Japanese quince (Chaenomeles japonica, JQ) press residue, offering a partial utilization of valuable bioactive compounds of wine industry by-products. To study the JQ oil extract yield, composition and oxidation stability, we modified the co-solvent composition during the supercritical CO2 (SC-CO2) extraction of oil by adding different ethanol content. The remaining defatted material was used for the isolation of proteins. The SC-CO2 extraction yielded oil rich in polyunsaturated fatty acids, tocopherols, and phytosterols. The use of ethanol as a co-solvent increased the oil yield but did not enhance its oxidative stability or content of antioxidants. We recovered protein isolate after removing tannins with 70% ethanol extraction in the next step. The JQ protein isolate contained all essential amino acids. In addition to its balanced amino acid composition, the protein isolate exhibited excellent emulsifying properties highlighting its potential as a food additive. In conclusion, JQ wine by-products can be utilized for the extraction of oil and protein fractions which can be used in food or cosmetic product formulation.

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Three types of extraction were used to obtain biologically active substances from the heartwood of M. amurensis: supercritical CO2 extraction, maceration with EtOH, and maceration with MeOH. The supercritical extraction method proved to be the most effective type of extraction, giving the highest yield of biologically active substances. Several experimental conditions were investigated in the pressure range of 50-400 bar, with 2% of ethanol as co-solvent in the liquid phase at a temperature in the range of 31-70 °C. The most effective extraction conditions are: pressure of 100 bar and a temperature of 55 °C for M. amurensis heartwood. The heartwood of M. amurensis contains various polyphenolic compounds and compounds of other chemical groups with valuable biological activity. Tandem mass spectrometry (HPLC-ESI-ion trap) was applied to detect target analytes. High-accuracy mass spectrometric data were recorded on an ion trap equipped with an ESI source in the modes of negative and positive ions. The four-stage ion separation mode was implemented. Sixty-six different biologically active components have been identified in M. amurensis extracts. Twenty-two polyphenols were identified for the first time in the genus Maackia.

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For improving the management of the production chain of PGI Mantua pears (which comprises many varieties, including Abate Fetel), applying the cardinal principles of circular economy and sustainability, the fruits with diseases or defects were recovered for producing dried rounds of pears from the Abate Fetel cultivar, a new product with high nutritional value that extends the remaining life. This process led to the production of secondary and residual by-products, which are mainly composed of the highest and lowest part of the fruits, comprising seeds, pulps, peels and petioles. Hence, this study was focused on the valorization of these secondary by-products of Abate Fetel pears through the production of pear extracts using traditional and "green" extraction methods that involve the use of supercritical CO2 fluid extraction. The produced extracts, together with a reference solvent-derived extract, were analyzed by HPLC-ESI-MS, and in parallel, their direct and cellular antioxidant activity were assessed. Evidence has indicated that all the tested extracts reduced the H2O2-induced reactive oxygen species (ROS), lipid peroxidation and nitric oxide (NO) levels, respectively, in human intestinal Caco-2 cells. Hence, this study clearly suggests that extracts obtained from Mantuan PGI pear by-products may be used as valuable sources of bioactive upcycled phytocomplex for the development of dietary supplements and/or functional foods.

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In this research, we have reported the valorization possibilities of Matricaria recutita white ray florets using supercritical fluid extraction (SFE) with CO2. Experiments were conducted at temperatures of 35-55 °C and separation pressures of 5-9 MPa to evaluate their impact on the chemical composition and biological activity of the extracts. The total obtained extraction yields varied from 9.76 to 18.21 g 100 g-1 DW input. The greatest extraction yield obtained was at 9 MPa separation pressure and 55 °C in the separation tank. In all obtained extracts, the contents of total phenols, flavonoids, tannins, and sugars were determined. The influence of the supercritical CO2 extraction conditions on the extract antioxidant capacity was evaluated using the quenching activity of 2,2-diphenyl-1-picrylhydrazyl (DPPH). The chemical composition of the extracts was identified using both gas and liquid chromatography-mass spectrometry methods, whereas analyses of major and minor elements as well as heavy metals by microwave plasma atomic emission spectrometer were provided. Moreover, extracts were compared with respect to their antimicrobial activity, as well as the cytotoxicity and phototoxicity of the extracts. The results revealed a considerable diversity in the phytochemical classes among all extracts investigated in the present study and showed that the Matricaria recutita white ray floret by-product possesses cytotoxic and proliferation-reducing activity in immortalized cell lines, as well as antimicrobial activity. To the best of our knowledge, this is the first paper presenting such comprehensive data on the chemical profile, antioxidant properties, and biological properties of SFE derived from Matricaria recutita white ray florets. For the first time, these effects have been studied in processing by-products, and the results generated in this study provide valuable preconditions for further studies in specific test systems to fully elucidate the mechanisms of action and potential applications, such as potential use in cosmetic formulations.

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Black pepper (P. nigrum L.) is considered one of the most valuable spices and a promising candidate in natural product research. In this study, the influence of different combinations of pressures (100-300 bar) and temperatures (40-60 °C) on the supercritical CO2 (SC-CO2) recovery of several key compounds from black pepper was evaluated systematically. The extraction curves showed that terpenes were recovered in a short time under all studied conditions. In contrast, higher pressure values were required to extract piperamides efficiently. Furthermore, the differences in the extraction kinetics of piperine, piperettine, pellitorine, guineensine, and N-isobutyl-2,4,14-eicosatrienamide were linked with several structural features, such as the nature of the amine group or the terminal part of the fatty acid. The data from the isocratic experiments represented the starting point for designing a two-step pressure gradient SC-CO2 process in which one terpene-rich and one piperamide-rich product were successively obtained.

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Amongst the current alternatives, algae were proven to be a promising source of biofuel, which is renewable and capable of meeting world demand for transportation fuels. However, a suitable lipid extraction method that efficiently releases the lipids from different algal strains remains a bottleneck. The multifarious pretreatment methods are prevalent in this field of lipid extraction, and therefore, this article has critically reviewed the various lipid extraction methods for ameliorating the lipid yield from algae, irrespective of the strains/species. Physical, mechanical, and chemical are the different types of pretreatment methods. In this review, methodologies such as homogenization, sonication, Soxhlet extraction, microwave treatment, and bead-beating, have been studied in detail and are the most commonly used methods for lipid extraction. Specific advanced/emerging processes such as supercritical CO2 extraction, ionic liquid, and CO2 switchable solvent-based algal lipid extraction are yet to be demonstrated at pilot-scale, though promising. The extraction of lipids has to be financially conducive, environmentally sustainable, and industrially applicable for further conversion into biodiesel. Hence, this paper discusses variable pretreatment for lipid extraction and imparts a comparative analysis to elect an efficient, economically sound lipid extraction method for pilot-scale biodiesel production.

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This work investigates the prospects for exploitation of Gnaphalium viscosum (Kunth) abundant but with limited applications till present biomass. The feasibility of traditional techniques (two-phase solvent, and the benchmark Soxhlet extraction) and supercritical extraction without/with a cosolvent at T = 40-60 °C and p = 30-50 MPa was examined to explore the possibility of recovering phytochemicals from G. viscosum leaves, flowers and stems. The efficiency of the techniques was assessed and compared based on yield, influence of solvents used, total phenolic content and antioxidant activity of the extracts. Phenolics of different complexities were identified and quantified by applying LC (LC-MS/MS, and LC-HRAM), while the fatty acid profile was determined by GC-FID. The results of this extensive study demonstrated the huge valorization potential and prospects of G. viscosum, since highly potent antioxidants such as kaempferol, kaempferol-3-O-ß-d-glucoside (astragalin), and chlorogenic acid were ascertained in considerable amounts. Furthermore, for the first time, the presence of leontopodic acid, a greatly substituted derivative of glucaric acid, was detected in the species.

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The employment of supercritical carbon dioxide extraction for obtaining the chemical compounds from N. tabacum leaves, especially nicotine, is advancing. The supercritical carbon dioxide extraction of dried N. tabacum cv. Samsun and N. tabacum cv. Virginia at different process parameters was performed to obtain the highest extraction yield and nicotine relative amount. The optimal extraction conditions concerning the highest extraction yield and nicotine relative amount were determined by response surface methodology. The highest extraction yield for N. tabacum cv. Samsun was 2.99% and for N. tabacum cv. Virginia 2.33% at 23.41 MPa, 50 °C and 90 min of extraction time. The highest nicotine relative amount in N. tabacum cv. Samsun and N. tabacum cv. Virginia was at 15 MPa, 50 °C and 90 min extraction time and was 242.1 mg per 100 g of plant material and 32.4 mg per 100 g of plant material, respectively. The pressure, temperature and time influenced the extraction yield and nicotine relative amount recovery in N. tabacum cv. Samsun and N. tabacum cv. Virginia. A general inclusive concept in respect to pressure, temperature and time of the supercritical carbon dioxide extraction and a report on phytochemicals present in two N. tabacum varieties is presented.

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In the recent years, edible brown seaweed, Undaria pinnatifida, has presented beneficial effects, which may be correlated with this species containing major bioactive compounds, such as carotenoids, fatty acids, and phytosterols. Marine carotenoid fucoxanthin is abundantly present in edible Undaria pinnatifida and features strong bioactive activities. The stem of Undaria pinnatifida is very hard to gnaw off and cannot be swallowed; therefore, it is usually discarded as waste, making it an environmental issue. Hence, making full use of the waste stem of Undaria pinnatifida is an urgent motivation. The present study aims to explore the optimal preparation technology of fucoxanthin from Undaria pinnatifida stems using supercritical carbon dioxide methods and provides approaches for the extraction and preparation of bioactive compounds from a waste seaweed part. With the comprehensive optimization conditions applied in this study, the experimental yield of fucoxanthin agreed closely with the predicted value by > 99.3%. The potential of α-amylase and glucoamylase to inhibit bioactive compounds was evaluated. The results demonstrated that the inhibition activity (IC50 value) of α-amylase (0.1857 ± 0.0198 µg/ml) and glucoamylase (0.1577 ± 0.0186 µg/ml) varied with extraction conditions due to the different contents of bioactive components in the extract, especially fucoxanthin (22.09 ± 0.69 mg/g extract). Therefore, this study confirmed supercritical fluid extraction technology to be a useful sample preparation method, which can effectively be used to prepare fucoxanthin from waste marine resources. This method can potentially be applied in functional food and related industries.

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Natural products are increasingly in demand in dermatology and cosmetology. In the present study, highly valuable supercritical CO2 (sCO2) extracts rich in bioactive compounds with antiradical and antibacterial activity were obtained from the inflorescences of industrial hemp. Volatile compounds were analyzed by gas chromatography in tandem with mass spectrometry (GC-MS), while cannabinoids were determined by high performance liquid chromatography (HPLC-DAD). Extraction yields varied from 0.75 to 8.83%, depending on the pressure and temperature applied. The extract obtained at 320 bar and 40 °C with the highest content (305.8 µg mg-1) of cannabidiolic acid (CBDA) showed the best antiradical properties. All tested extract concentrations from 10.42 µg mL-1 to 66.03 µg mL-1 possessed inhibitory activities against E. coli, P. aeruginosa, B. subtilis, and S. aureus. The sCO2 extract with the highest content of cannabidiol (CBD) and rich in α-pinene, ß-pinene, ß-myrcene, and limonene was the most effective. The optimal conditions for sCO2 extraction of cannabinoids and volatile terpenes from industrial hemp were determined. The temperature of 60 °C proved to be optimal for all responses studied, while the pressure showed a different effect depending on the compounds targeted. A low pressure of 131.2 bar was optimal for the extraction of monoterpenes, while extracts rich in sesquiterpenes were obtained at 319.7 bar. A high pressure of 284.78 bar was optimal for the extraction of CBD.

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The essential oil extracted from Cinnamomum camphora leaves is a mixture of volatile compounds, mainly terpenes, and is widely used in medicine, perfume and chemical industries. In this study, the extraction processes of essential oil from Cinnamomum camphora leaves by steam distillation and supercritical CO2 extraction were summarized and compared, and the camphor tree essential oil was detected by GC/MS. The extraction rate of essential oil extracted by steam distillation is less than 0.5%, while that of supercritical CO2 extraction is 4.63% at 25 MPa, 45 °C and 2.5 h. GC/MS identified 21 and 42 compounds, respectively. The content of alcohols in the essential oil is more than 35%, and that of terpenoids is more than 80%. The steam extraction method can extract volatile substances with a low boiling point and more esters and epoxides; The supercritical method is suitable for extracting weak polar substances with a high alcohol content. Supercritical CO2 extraction can selectively extract essential oil components and effectively prevent oxidation and the escape of heat sensitive substances.

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Lycopene, ß-carotene and ω-fatty acids are major compounds in tomatoes with known antioxidant activity, capable of preventing health disorders. The identification of potential natural sources of antioxidants, extraction efficiencies and antioxidant activity assessments are essential to promote such products to be used in the food, pharmaceutical or cosmetic industries. This work presents four added-value products recovered from tomatoes: pigmented solid oleoresin, pigmented oil and two raw extracts from supercritical and Soxhlet extraction. Different parameters including the matrices of tomatoes, extraction methods, green solvents and operating parameters were varied to obtain extracts with different qualities. Extract analysis was performed using UV-VIS, FT-IR, GC-MS, Folin-Ciocalteu and DPPH methods. The highest-quality extract was the solid oleoresin obtained from pomace using supercritical CO2 extraction at 450 bar, 70 °C and 11 kg/h: 1016.94 ± 23.95 mg lycopene/100 g extract, 154.87 ± 16.12 mg ß-carotene/100 g extract, 35.25 ± 0.14 mg GAE/g extract and 67.02 ± 5.11% inhibition DPPH. The economic feasibility of the three extraction processes (1:10:100 kg dried pomace/batch as scalability criterion) was evaluated. The most profitable was the supercritical extraction process at the highest capacity, which produces pigmented solid oleoresin and oil with high content of lycopene valorized with a high market price, using natural food waste (pomace).

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In this study, the volatile compound profiles of gurum seed oil were determined using two methods: supercritical CO2 extraction (SFE) and the screw press process (SPP). For volatile compounds extraction and identification, headspace solid-phase micro-extraction (HS-SPME) and GC-MS were used, respectively. A total number of 56 volatile compounds were revealed and identified in oil extracted by SFE, while only 40 compounds were detected in extracted oil by SPP. Acids, aldehydes, esters, ketones, furans, and other components were present in the highest ratio in oil extracted by SFE. In contrast, alcohols and alkenes were found in the highest proportion in oil extracted by SPP. In this study, it was observed that SFE showed an increase in the amounts of volatile compounds and favorably impacted the aroma of gurum seed oil. The results reveal that different extraction methods significantly impact the volatile components of gurum seed oil, and this study can help evaluate the quality of the oil extracted from gurum seeds.

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