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By-products of essential oils (EOs) in the industry represent an exploitable material for natural and safe antioxidant production. One representative group of such by-products is distilled solid residues, whose composition is properly modulated by the distillation method applied for the recovery of EOs. Recently, in terms of Green Chemistry principles, conventional extraction and distillation processes are considered outdated and tend to be replaced by more environmentally friendly ones. In the present study, microwave-assisted hydro-distillation (MAHD) was employed as a novel and green method for the recovery of EOs from three aromatic plants (rosemary, Greek sage and spearmint). The method was compared to conventional ones, hydro-distillation (HD) and steam-distillation (SD), in terms of phytochemical composition of distilled solid residues, which was estimated by spectrophotometric and chromatographic methods. Total phenolic content (TPC), total flavonoid content (TFC) and antioxidant activity (ABTS, DPPH and FRAP) results highlighted the distilled solid residues as good sources of antioxidants. Moreover, higher antioxidant activity was achieved for MAHD extracts of solid residues in comparison to HD and SD extracts. A metabolomics approach was carried out on the methanolic extracts of solid residues obtained by different distillation methods using LC-MS analysis followed by multivariate data analysis. A total of 29 specialized metabolites were detected, and 26 of them were identified and quantified, presenting a similar phenolic profile among different treatments, whereas differences were observed among different species. Rosmarinic acid was the most abundant phenolic compound in all extracts, being higher in MAHD extracts. In rosemary and Greek sage extracts, carnosol and carnosic acid were quantified in significant amounts, while trimers and tetramers of caffeic acid (salvianolic acids isomers) were identified and quantified in spearmint extracts, being higher in MAHD extracts. The obtained results pointed out that MAHD extracts of distilled solid by-products could be a good source of bioactives with potential application in the food, pharmaceutical and cosmetic industries, contributing to the circular economy.

The present study optimized pre-treatment conditions for bioenzyme-mediated hydro-distillation (BMHD) for extraction of mint oil from mentha leaves and the results were compared with those of traditional hydro-distillation (HD) method using response surface methodology. The bio-enzymes produced from moringa leaves had maximum pectinase activity (287.04 µg of sugar/min/ml) followed by xylanase (87.78 µg of sugar/min/ml) while endoglucanase, exoglucanase and amylase activities were comparatively low. The optimized conditions for HD were 69.08 temperature for 173.70 min with water:sample of 10.0. The optimized conditions for enzyme pre-treatment of mentha leaves by BMHD were enzyme concentration of 8%, for a period of 120 min at an incubation period of 40 ℃. The yield (%) and menthol content (%) of the oil at optimized conditions by HD were 1.55 ml/100 g of sample and 56.40% menthol content, respectively, and for BMHD the yield and menthol content (%) of the oil at optimized conditions were 3.69% and 72.80%, respectively. It was found that BMHD leads to a 130% increase in the yield of mint oil and a 10% increase in menthol content as compared to the HD method. No significant difference in physical parameters was observed in mint oil extracted via both methods. Therefore, BMHD is a cost-effective and sustainable approach having an edge over the HD method without compromising the quality and could be a viable approach for commercial purposes.

Spearmint essential oil (SEO), one of the economically valuable natural products, has special importance in the food, pharmaceutical, and perfumery industries due to its antifungal, antioxidant, and enzyme inhibitory properties. In this study, we optimized and evaluated the effect of three pre‐treatments on the extraction of SEO for quantity and quality: ultrasonic bath (UB), water to material ratio‐ultrasonic bath (W/M‐UB), and cold plasma‐ultrasonic bath (CP‐UB). Three experiments were designed using the central composite design (CCD) of response surface methodology (RSM). Experimental treatments included UB temperature (30–80°C) and time duration (1–30 min), cold plasma (CP) power (15–24 kV), and water/material ratio (10–40). Then, SEOs were extracted by hydro‐distillation using the Clevenger apparatus. The results showed that SEO yield in the optimal conditions of treatments was 119.7%, 206.6%, and 155.7% higher in UB, W/M‐UB, and CP‐UB pretreatments respectively, in comparison to control sample and optimized conditions were UB temperature: 37.3°C and UB time: 5.2 min at UB treatment, 33.9 of W/M ratio, 69.9°C of UB temperature and 6.9 min of UB time at W/M‐UB treatment and CP power: 22.176, UB temperature: 40.135 and UB time: 24.122 at CP‐UB treatment. Oxygenated monoterpenes were also higher in the essential oils (EOs) of all three treated plant materials. In conclusion, the SEO extraction yield improved by the application of the pretreatments in optimized conditions. The aim of this study was to increase the extraction efficiency of essential oil. Treatments were ultrasonic bath, water to material ratio, and cold plasma. Increasing the time of ultrasonic bath and cold plasma power led to a higher yield. Treatments with ultrasonic bath temperature and water/material ratio inversely affected the yield. The treatments raised the percentage of oxygenated monoterpenes slightly.

A microwave distillation method was optimized for the extraction and isolation of cannabis essential oil from fresh and dried hemp inflorescences. The developed method enabled us to obtain a distilled product rich in terpenes and terpenoid compounds, responsible of the typical and unique smell of the cannabis plant. The distillate from different hemp cultivars, including Kompolti, Futura 75, Carmagnola, Felina 32 and Finola were characterized by using a gas chromatograph equipped with both mass spectrometer and flame ionization detectors. In a single chromatographic run, the identity and absolute amounts of distilled compounds were determined. Peak assignment was established using a reliable approach based on the usage of two identification parameters, named reverse match, and linear retention index filter. Absolute quantification (mg g−1) of the analytes was performed using an internal standard method applying the flame ionization detector (FID) response factors according to each chemical family. An enantio-GC-MS method was also developed in order to evaluate the enantiomeric distribution of chiral compounds, an analytical approach commonly utilized for establishing the authenticity of suspicious samples.

Oral disorders can exert systemic ramifications beyond their localized effects on dental tissues, implicating a wide array of physiological conditions. The utilization of essential oils (EOs) for protection of oral health represents a longstanding practice. Consequently, in this investigation, essential oil derived from Nigella sativa seeds (NSEO) underwent isolation via the hydro-distillation process, followed by a comprehensive evaluation of its antioxidant, anti-inflammatory, anti-fungal, antibacterial activities, and cytocompatibility. The isolated NSEO manifested as a pale-yellow substance and was found to harbor a diverse spectrum of bioactive constituents, including steroids, triterpenoids, flavonoids, phenols, proteins, alkaloids, tannin, sesquiterpenoid hydrocarbons, monoterpenoid alcohol, and monoterpenoid ketone (thymoquinone). Notably, the total phenolic content (TPC) and total flavonoid content (TFC) of NSEO were quantified at 641.23 μg GAE/gm and 442.25 μg QE/g, respectively. Furthermore, NSEO exhibited concentration-dependent inhibition of protein denaturation, HRBC membrane stabilization, and hemolysis inhibition. Comparative analysis revealed that NSEO and chlorhexidine (CHX) 0.2% displayed substantial inhibition of hemolysis compared to aspirin. While NSEO and CHX 0.2% demonstrated analogous antibacterial activity against Escherichia coli , Staphylococcus aureus , and Pseudomonas aeruginosa , NSEO showcased heightened efficacy against Lactobacillus acidophilus and Candida albicans . Additionally, NSEO exhibited pronounced effects against periodontal pathogens such as Aggregatibacter actinomycetemcomitans , Porphyromonas gingivalis , Tannerella forsythia , and Prevotella intermedia . Importantly, no cytotoxicity was observed on human gingival fibroblast cell lines. These findings underscore the potential of NSEO as a potent antibacterial and antifungal agent in the management of oral microbial pathogens, thereby offering avenues for the development of innovative therapies targeting diverse oral inflammatory conditions. Nevertheless, further investigations are imperative to unlock its full therapeutic repertoire.

Solvent-free microwave extraction (SFME) and conventional hydro-distillation (HD) were used for the extraction of essential oils (EOs) from Egyptian sweet basil (Ocimum basilicum L.) leaves. The two resulting EOs were compared with regards to their chemical composition, antioxidant, and antimicrobial activities. The EO analyzed by GC and GC-MS, presented 65 compounds constituting 99.3% and 99.0% of the total oils obtained by SFME and HD, respectively. The main components of both oils were linalool (43.5% SFME; 48.4% HD), followed by methyl chavicol (13.3% SFME; 14.3% HD) and 1,8-cineole (6.8% SFME; 7.3% HD). Their antioxidant activity were studied with the 2,2-diphenyl-1-picrylhydrazyl (DPPH•) radical scavenging method. The heating conditions effect was evaluated by the determination of the Total Polar Materials (TPM) content. The antimicrobial activity was investigated against five microorganisms: two Gram-positive bacteria, Staphylococcus aureus and Bacillus subtilis, two Gram-negative bacteria, Escherichia coli and Pseudomonas aeruginosa, and one yeast, Candida albicans. Both EOs showed high antimicrobial, but weak antioxidant, activities. The results indicated that the SFME method may be a better alternative for the extraction of EO from O. basilicum since it could be considered as providing a richer source of natural antioxidants, as well as strong antimicrobial agents for food preservation.

The exploration of cucumber waste as a potential biorefinery feedstock is reported. Initially, extractives (essential oils) were isolated from cucumber waste via vacuum microwave hydro-distillation (VMHD). The yield and quality of the extractive were compared with respect to traditional hydro-distillation (HD). The essential oils were obtained over a range of microwave power (500, 750, 1000 W) and vacuum pressures (100, 200, 300 mbar). The highest quality (0.49 wt %) was obtained at a microwave irradiation power of 500 W and a vacuum of 300 mbar. VMHD is much quicker and more energy-efficient than HD. Within the context of a zero-waste biorefinery, the extractive-free residues were the solid residues from two different extraction methods were compared and characterized by ATR-IR, 13C solid-state NMR spectroscopy, SEM, TGA, and CHN elemental analysis. The resultant residues are cellulosic-rich, and no significant changes were observed with VMHD and HD treatment. The results indicated that the utilization of these residues can provide an efficient, inexpensive, and environment-friendly platform for the production of cellulosic materials.

The food industry uses essential oils derived from natural sources as flavouring and preservatives. The purpose of this study is to investigate how temperature affects the essential oil extracted from Trachyspermum ammi, seeds which has the best antioxidant and antimicrobial properties, in order to find a green substitute for toxic chemically produced preservatives used in food and pharmaceutical chemistry. Trachyspermum ammi (ajwain seeds) seeds were hydrodistilled at various temperatures (60°C to 90°C). The amount of essential oil was found to decrease on increasing temperature (2.1ml, 1.5 ml and 1.0 ml at 70°C, 80°C, and 90°C respectively). Hence, 70°C was the ideal temperature for extracting the essential oil from ajwain seeds. 25 components were discovered in the essential oil extracted from ajwain seeds by GC-MS technique. The predominant ingredient was shown to be thymol (31.40%). The percentages of scavenger activity against hydrogen peroxide were 70.75%, 86.99%, and 95.28% for 70°C, 80°C, and 90°C respectively. Due to the presence of the largest concentration of thymol (67.66%), the results showed that essential oil extracted at 90°C demonstrated the highest level of antioxidant property. By using the disc diffusion method, the antimicrobial activity of an essential oil made from ajwain seeds was evaluated. MIC50 of standard essential oil of Trachyspermum ammi seeds against gram positive strain was observed 10 µL/mL of culture and 25µL/mL of culture was observed against gram negative bacteria. Essential oil extracted at 70°C showed antimicrobial activity by forming zones of inhibition with diameters including discs of 18.3 mm and 14.36 mm against S. aureus and E. coli, respectively. Essential oil extracted at 80°C produced zones of inhibition with diameters of 18.68 mm and 15.30 mm, respectively. In the case of essential oil extracted at 90°C, the zones of inhibition against S. aureus and E. coli had diameters of 18.690.3 mm and 15.38 mm, respectively. As a result, using Trachyspermum ammi essential oil as a food preservative and the temperature at which it is extracted are unaffected by an increase in extraction temperature. Hence, essential oil obtained from Trachyspermum ammi seeds can be used as green alternative of chemically synthesized toxic preservatives used in food and pharmaceutical chemistry.

Waste or by-product use is in focus for reducing the environmental threat and acquiring wealth out of waste. The current study aim was to investigate the effects of ultrasound pretreatment on the extraction of bioactive compounds and composition of essential oils extracted from citrus waste. The response surface methodology (RSM) was used to optimize higher yield extraction parameters. Pretreatment of ultrasound-assisted extraction recovered 33% enhanced yield with reduced time and was economical as compared to conventional hydro-distilled process. The functional quality of essential oil was determined using FTIR and GC-MS. Antioxidants from citrus peel and pulp/pomace were extracted and analyzed by spectroscopic techniques. The quantification of bioactive compounds from citrus waste was performed using high performance liquid chromatography (HPLC). Mass transfer rate of antioxidants from peel and pomace were 30% increased as a result of ultrasound-assisted treatment. The significantly (p ≤ 0.05) higher TPC (735.54 mg/100 g) and antioxidant activity (44.26%) was recorded in Citrus sinensis Pulp and peel respectively. The bioactive compounds such as hesperidin (31.52 mg/100 g) was significantly higher in (p ≤ 0.05) in Citrus sinensis pulnd extract. Vanillin was found 1.21 mg/100 g in peel extract of citrus fruit, moreover vanillin was not detected in pulp extract. Myrecitin was not detected in both the samples. The bioactive natural compounds extracted from citrus peel can be used in food and pharma sector as natural anti-oxidantcompounds.

Feijoa is an aromatic fruit and the essential oil from feijoa peel could be a valuable by-product in the juicing industry. An initial comparison of the essential oil extraction methods, steam-distillation and hydro-distillation, was conducted. The volatile compounds in the essential oils from four feijoa cultivars were identified and semi-quantified by GC-MS and the aroma active compounds in each essential oil were characterized using SPME-GC-O-MS. Hydro-distillation, with a material to water ratio of 1:4 and an extraction time of 90 min, was the optimized extraction method for feijoa essential oil. The Wiki Tu cultivar produced the highest essential oil yield among the four selected cultivars. A total of 160 compounds were detected, among which 90 compounds were reported for the first time in feijoa essential oils. Terpenes and esters were dominant compounds in feijoa essential oil composition and were also major contributors to feijoa essential oil aroma. Key aroma active compounds in feijoa essential oils were α-terpineol, ethyl benzoate, (Z)-3-hexenyl hexanoate, linalool, (E)-geraniol, 2-undecanone, 3-octanone, α-cubebene, and germacrene D. This is the first report on the optimization of the extraction method and the establishment of the aroma profile of feijoa essential oils, with a comparison of four New Zealand grown cultivars.