Green Extraction Approach for Isolation of Bioactive Compounds in Wild Thyme (Thymus serpyllum L.) Herbal Dust-Chemical Profile, Antioxidant and Antimicrobial Activity and Comparison with Conventional Techniques.

The aim of this study was to provide a chemical profile and determine the antioxidant and antimicrobial activity of the essential oil (EO) and lipid extracts of Thymus serpyllum L. herbal dust obtained via conventional (hydrodistillation (HD) and Soxhlet extraction (SOX)) and novel extraction techniques (supercritical fluid extraction (SFE)). In addition, a comparative analysis of the chemical profiles of the obtained EO and extracts was carried out, as well as the determination of antioxidant, antibacterial and antifungal activity of the lipid extracts. According to the aforementioned antioxidant and antimicrobial activities and the monoterpene yield and selectivity, SFE provided significant advantages compared to the traditional techniques. In addition, SFE extracts could be considered to have great potential in terms of their utilization in the pharmaceutical and cosmetic industries, as well as appropriate replacements for synthetic additives in the food industry.

New Biological and Chemical Insights into Optimization of Chamomile Extracts by Using Artificial Neural Network (ANN) Model.

Chamomile is one of the most consumed medicinal plants worldwide. Various chamomile preparations are widely used in various branches of both traditional and modern pharmacy. However, in order to obtain an extract with a high content of the desired components, it is necessary to optimize key extraction parameters. In the present study, optimization of process parameters was performed using the artificial neural networks (ANN) model using a solid-to-solvent ratio, microwave power and time as inputs, while the outputs were the yield of the total phenolic compounds (TPC). Optimized extraction conditions were as follows: a solid-to-solvent ratio of 1:80, microwave power of 400 W, extraction time of 30 min. ANN predicted the content of the total phenolic compounds, which was later experimentally confirmed. The extract obtained under optimal conditions was characterized by rich composition and high biological activity. Additionally, chamomile extract showed promising properties as growth media for probiotics. The study could make a valuable scientific contribution to the application of modern statistical designs and modelling to improve extraction techniques.

Kinetics of Microwave-Assisted Extraction Process Applied on Recovery of Peppermint Polyphenols: Experiments and Modeling.

The aim of this work was to investigate the microwave-assisted extraction (MAE) kinetics of polyphenolic compounds from organic peppermint leaves. The phytochemicals of peppermint (Mentha piperita L.) are increasingly used in food technology due to their numerous biological activities. The processing of various plant materials by MAE and the production of high-quality extracts is becoming increasingly important. Therefore, the influence of microwave irradiation power (90, 180, 360, 600, and 800 W) on total extraction yield (Y), total polyphenols yield (TP), and flavonoid yield (TF) were investigated. Common empirical models (first-order, Peleg's hyperbolic, Elovich's logarithmic, and power-law model) were applied to the extraction process. The first-order kinetics model provided the best agreement with the experimental results in terms of statistical parameters (SSer, R2, and AARD). Therefore, the influences of irradiation power on the adjustable model parameters (k and Ceq) were investigated. It was found that irradiation power exerted a significant influence on k, while its influence on the asymptotic value of the response was negligible. The highest experimentally determined k (2.28 min-1) was obtained at an irradiation power of 600 W, while the optimal irradiation power determined by the maximum fitting curve determination predicted the highest k (2.36 min-1) at 665 W.

Antimicrobial potential of kombucha fresh cheese with the addition of sage (Salvia officinalis L.) and its preparations.

One of the main challenges in fresh cheese technology is its rather limited shelf life. Prolongation of the shelf life of fresh cheese has been the focus of numerous research studies and different strategies have been thus used. One of the strategies that could prolong the shelf life of fresh cheese, as well as increase its quality is the application of different starter cultures. As the antimicrobial capacity of sage (Salvia officinalis) has been proven, the possibility of reusing its by-product obtained from a tea factory could be a significant step towards the retention of environmental equilibrium and simultaneous production of food with additional functional value. Therefore, the aim of our research was to examine the antimicrobial potential of kombucha fresh cheese with the addition of ground herbal sage, sage essential oil and sage supercritical fluid extract, and compare it with fresh cheese obtained from a commercial starter culture. In order to examine the antimicrobial activity of kombucha fresh cheese produced with the addition of sage preparations, the produced samples were artificially contaminated with common foodborne contaminants: Listeria monocytogenes, Escherichia coli and Staphylococcus aureus. The obtained results revealed that the addition of sage essential oil and herbal ground sage increased the antimicrobial activity during the 30 days of storage against E. coli in kombucha fresh cheese (decrease of 2.9 and 2.5 log CFU g-1, respectively). Implementation of sage significantly increased the antimicrobial activity of the fresh cheese produced with a commercial XPL-1 starter culture against L. monocytogenes (essential oil - 0.9 log CFU g-1 and ground sage - 1.2 log CFU g-1). In the XPL-1 sample, the growth of S. aureus was inhibited by the addition of ground sage - a decrease of 1.4 log CFU g-1. Analysis of the total phenols revealed their 5-fold higher content in the kombucha fresh cheeses compared to the samples obtained by the XPL-1 starter culture. These results correlate with the higher antimicrobial activity of the kombucha fresh cheese samples compared to the XPL-1 samples. According to our results, industrial waste, obtained as a by-product in sage (Salvia officinalis) filter tea production, can be efficiently used in fresh cheese technology in order to increase the antimicrobial activity against L. monocytogenes, E. coli and S. aureus.

Recovery of Polyphenolic Compounds and Vitamins from the Stinging Nettle Leaves: Thermal and Behavior and Biological Activity of Obtained Extracts.

Stinging nettle (SN) is an extraordinary plant from the Urticaceae botanical family. It is well-known and widely used in food and folk medicine to treat different disorders and diseases. This article aimed to study the chemical composition of SN leaves extracts, i.e., polyphenolic compounds and vitamins B and C, because many studies ascribed high biological potency to these compounds and their significance in the human diet. Besides the chemical profile, the thermal properties of the extracts were studied. The results confirmed presence of many polyphenolic compounds and vitamins B and C. It also showed that the chemical profile closely correlated with the applied extraction technique. The thermal analysis showed that analyzed samples were thermally stable up to about 160 °C. Thermal degradation of samples UAE, MAE, and MAC took place in four steps, and sample SE in three steps. Altogether, results confirmed the presence of health-beneficial compounds in stinging nettle leaves and indicated the possible application of its extract in pharmaceutical and food industries as both a medicinal and food additive.

Isolation, Bioactive Potential, and Application of Essential Oils and Terpenoid-Rich Extracts as Effective Antioxidant and Antimicrobial Agents in Meat and Meat Products.

Using food additives (e.g., preservatives, antioxidants) is one of the main methods for preserving meat and meat product quality (edible, sensory, and technological) during processing and storage. Conversely, they show negative health implications, so meat technology scientists are focusing on finding alternatives for these compounds. Terpenoid-rich extracts, including essential oils (EOs), are remarkable since they are generally marked as GRAS (generally recognized as safe) and have a wide ranging acceptance from consumers. EOs obtained by conventional or non-conventional methods possess different preservative potentials. Hence, the first goal of this review is to summarize the technical-technology characteristics of different procedures for terpenoid-rich extract recovery and their effects on the environment in order to obtain safe, highly valuable extracts for further application in the meat industry. Isolation and purification of terpenoids, as the main constituents of EOs, are essential due to their wide range of bioactivity and potential for utilization as natural food additives. Therefore, the second goal of this review is to summarize the antioxidant and antimicrobial potential of EOs and terpenoid-rich extracts obtained from different plant materials in meat and various meat products. The results of these investigations suggest that terpenoid-rich extracts, including EOs obtained from several spices and medicinal herbs (black pepper, caraway, Coreopsis tinctoria Nutt., coriander, garlic, oregano, sage, sweet basil, thyme, and winter savory) can be successfully used as natural antioxidants and antimicrobials in order to prolong the shelf-life of meat and processed meat products. These results could be encouraged for higher exploitation of EOs and terpenoid-rich extracts in the meat industry.

Recovery of Biologically Active Compounds from Stinging Nettle Leaves Part II: Processing of Exhausted Plant Material after Supercritical Fluid Extraction.

Stinging nettle (Urtica dioica L.) is one fantastic plant widely used in folk medicine, pharmacy, cosmetics, and food. This plant's popularity may be explained by its chemical composition, containing a wide range of compounds significant for human health and diet. This study aimed to investigate extracts of exhausted stinging nettle leaves after supercritical fluid extraction obtained using ultrasound and microwave techniques. Extracts were analyzed to obtain insight into the chemical composition and biological activity. These extracts were shown to be more potent than those of previously untreated leaves. The principal component analysis was applied as a pattern recognition tool to visualize the antioxidant capacity and cytotoxic activity of extract obtained from exhausted stinging nettle leaves. An artificial neural network model is presented for the prediction of the antioxidant activity of samples according to polyphenolic profile data, showing a suitable anticipation property (the r2 value during the training cycle for output variables was 0.999).

Essential Oils from Apiaceae, Asteraceae, Cupressaceae and Lamiaceae Families Grown in Serbia: Comparative Chemical Profiling with In Vitro Antioxidant Activity.

The aim of the present study was to investigate the chemical profile and antioxidant activity of essential oils obtained from the most commonly grown plant species in Serbia. Aromatic and medicinal plants from Lamiaceae (Mentha x Piperita, Ocimum basilicum, Origanum majorana, Origanum vulgare, Salvia officinalis, Satureja hortensis, Satureja montana and Thymus vulgaris), Asteraceae (Ehinacea purpurea and Matricaria chamomilla), Apiaceae (Anethum graveolens, Carum carvi, Foeniculum vulgare, Petroselinum crispum and Pimpinella anisum) and Cupressaceae (Juniperus comunis) were selected as raw material for essential oils (EOs)' isolation. Hydrodistillation (HD) was used for the isolation of EOs while they were evaluated in terms of yield and terpenoid profiles by GC-MS. In vitro radical scavenging DPPH and ABTS+ radical activities were carried out for all EOs. Finally, a principal component analysis (PCA) was performed with the experimental results of the composition and antioxidant activity of the EOs, which showed a clear distinction between the selected plant species for the aforementioned responses. This work represents a screening tool for the selection of other EO candidates for further processing by emerging extraction techniques and the use of EOs as natural additives for meat products.

Antibacterial Activity of Selected Essential Oils against Foodborne Pathogens and Their Application in Fresh Turkey Sausages.

Essential oils (EOs) isolated from different plant materials, namely Origanum majorana L., Satureja hortensis L., and Satureja montana L. (OMEO, SHEO, and SMEO, respectively), were used in fresh turkey sausage processing. The chemical composition and in vitro antimicrobial potential of selected EOs and their mixture were determined. The minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) against foodborne pathogens (Escherichia coli, Salmonella Enteritidis, and Listeria monocytogenes) ranged in the interval of 0.44-7.1 µL/mL. Fresh turkey sausages were produced with EOs addition and marked as follows: TOMEO-0.150 µL/g OMEO; TSHEO-0.150 µL/g SHEO; TSMEO-0.150 µL/g SMEO; TEOM-0.050 µL/g OMEO, 0.050 µL/g SHEO and 0.050 µL/g SMEO, and control (C) (without EOs). Microbiological profile and biogenic amines content in fresh turkey sausages were recorded during storage. The selected EOs and their mixture efficiently reduced bacterial growth and biogenic amines formation and accumulation. The lowest Enterobacteriaceae count and total biogenic amine (BA) concentration were determined through treatment TSHEO. The results of this study show that selected EOs could be useful in fresh turkey sausage processing in order to improve safety and shelf-life.

Isolation of Garlic Bioactives by Pressurized Liquid and Subcritical Water Extraction.

Garlic (Allium sativum L.) is widely used in various food products and traditional medicine. Besides unique taste and flavour, it is well known for its chemical profile and bioactive potential. The aim of this study was to apply subcritical water extraction (SWE) and pressurized liquid extraction (PLE) for the extraction of bioactive compounds from the Ranco genotype of garlic. Moreover, PLE process was optimized using response surface methodology (RSM) in order to determine effects and optimize ethanol concentration (45-75%), number of cycles (1-3), extraction time (1-3 min) and temperature (70-110 °C) for maximized total phenols content (TP) and antioxidant activity evaluated by various in vitro assays. Furthermore, temperature effect in SWE process on all responses was evaluated, while allicin content (AC), as a major organosulphur compound, was determined in all samples. Results indicated that PLE provided tremendous advantage over SWE in terms of improved yield and antioxidant activity of garlic extracts. Therefore, high-pressure processes could be used as clean and green procedures for the isolation of garlic bioactives.

The Effect of Humidity on the Dissolution Kinetics and Tablet Properties of Immediate-Release Tablet Formulation Containing Lamotrigine.

This study aims to find the effects of high (75%) and low (30%) humidity conditions and its correlation with formulation composition on dissolution kinetics of lamotrigine (LMT) from prepared immediate-release tablets during one- and four-week periods. Two types of fillers microcrystalline cellulose (MCC) or anhydrous lactose (LAC), disintegrant sodium starch glycolate (NaSG, 0.5% or 4%), and lubricant magnesium stearate (MgST, 0.25% or 5%) were used. A three-factor two-stage complete factorial design (23) was used to assess the influence of the composition of the tested formulations. The tablets were produced by direct compression and characterized using a disintegration test, a resistance to crushing test, and dissolution tests (pH 1.2 and pH 6.8). Using Design Expert software, it was concluded that in addition to the effect of fillers on pH 6.8, NaSG has a significant impact after exposure to high and low humidity, as well as its interaction with LAC and MCC. In the dissolution medium pH 1.2, under conditions of high humidity, the content of MgST and NaSG and their interaction show a significant influence. The release rate of LMT was affected by humidity as well as type of excipients and their interactions.

Polyphenols Recovery from Thymus serpyllum Industrial Waste Using Microwave-Assisted Extraction-Comparative RSM and ANN Approach for Process Optimization.

The aim of this study was to valorize Thymus serpyllum L. herbal dust, the particular fraction distinguished as industrial waste from filter-tea production. This work demonstrated comparable analysis considering model fitting, influence analysis and optimization of microwave-assisted extraction (MAE) of bioactive compounds from the aforementioned herbal dust using face-centered central composite experimental design within the response surface methodology (RSM), as well as artificial neural networks (ANN). In order to increase yield and amount of compounds of interest and minimize solvent, time and energy consumption, the ethanol concentration (45, 60 and 75%), extraction time (5, 12.5 and 20 min), liquid-solid ratio (10, 20 and 30 mL/g) and irradiation power (400, 600 and 800 W) were used as independent variables. Total extraction yield (Y), total phenols yield (TP), as well as antioxidant activity parameters obtained by DPPH and ABTS assays, were selected as responses. It could be concluded that the MAE technique is an efficient approach for the extraction of biologically active compounds from T. serpyllum herbal dust, which represents a high-value source of natural antioxidants with great potential for further use in various forms within different branches of industry.

Antioxidative capacity of fresh kombucha cheese fortified with sage herbal dust and its preparations.

Recent studies have intensively investigated the possibility of kombucha application as non-conventional starter culture in manufacture of various fermented dairy products. Furthermore, natural extracts from medicinal and aromatic plants contain different biologically active components which often have antioxidant properties. Based on the stated above, the aim of this research was to investigate the possibility of kombucha inoculum application as a new starter culture in fresh cheese technology, as well as to investigate effects of sage (Salvia officinalis) herbal dust (by-product from filter tea factory), its essential oil and supercritical fluid extract on antioxidative activity and sensory characteristics of produced fresh kombucha cheese during 10 days of storage. In all samples, higher ABTS than DPPH radical scavenging activity was determined. Freshly prepared and 10 days stored kombucha cheeses fortified with different types of sage preparations had significantly higher FRAP values than the control sample. All analysed samples had satisfied sensory characteristics and same scores of sensory evaluation after the production. Kombucha fresh cheese with addition of different types of sage preparations can be an innovative and valuable dairy product.

Isolation of Cherry Seed Oil Using Conventional Techniques and Supercritical Fluid Extraction.

This study aims to compare the suitability of three extraction techniques (cold pressing, Soxhlet and supercritical fluid extraction (SFE)) to isolate oil from cherry seeds. Oils were examined in terms of extraction yield, fatty acids profile, tocopherols yield and antioxidant activity. Additionally, influence of SFE parameters was evaluated using one-factor-at-a-time design with pressure (200−350 bar), temperature (40−70 °C), flow rate (0.2−0.4 kg/h) and particle size (<800 µm and >800 µm). Oil yields ranged from 2.50% to 13.02%, whereas the highest yield was achieved with SFE. Samples were rich in polyunsaturated fatty acids, regardless of the applied extraction technique. The main fatty acids were linoleic (46.32−47.29%), oleic (40.89−41.65%), palmitic (6.56−8.00%) and stearic (2.21−2.30%) acid. Total tocopherols yield was between 16.63 mg/100 g oil and 60.61 mg/100 g oil, and highest yield was achieved with SFE. Among the tocopherols, γ-tocopherol was the most abundant, followed by α-, δ- and ß-tocopherol. Antioxidant activity was determined using 1,1-diphenyl-2-picrylhydrazyl (DPPH) and 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic) cation (ABTS) assays, and the results indicated that SFE extracts exhibited better or comparable antioxidant potential compared to traditional techniques. The comparison between modern and conventional extractions for oil recovery demonstrates pros and cons for the possibility of industrial application.

Recovery of biologically active compounds from stinging nettle leaves part I: Supercritical carbon dioxide extraction.

Stinging nettle is annual plant from Urticaceae family used as food and medicine. Due to the nonsufficient data, this work aimed to isolate the bioactive compounds from the stinging nettle leaves by supercritical carbon dioxide. Extracts were analyzed and assessed for antioxidant and cytotoxic activities. Main fatty acids were α-linolenic (31.06-58.42 mg/g E), palmitic (9.17-13.12 mg/g E), and linoleic (10.93-16.51 mg/g E) acids. Chlorophylls (33.00-7365.11 mg/100 g E) and carotenoids (166.88-722.62 mg/100 g E) were also found in all samples. Four empirical kinetic equations were effectively utilized for kinetic modeling of supercritical fluid extraction. As per proper statistical features, empirical models show good concurrence with experimental data. The numerical modeling of a process is gainful to foresee the process conduct and furthermore extend the methodology from laboratory to industrial scales. The principal component analysis was used to visualize the fatty acids profile, antioxidant capacity, and cytotoxic activity of extract.

Supercritical Fluid Extraction Kinetics of Cherry Seed Oil: Kinetics Modeling and ANN Optimization.

This study was primarily focused on the supercritical fluid extraction (SFE) of cherry seed oil and the optimization of the process using sequential extraction kinetics modeling and artificial neural networks (ANN). The SFE study was organized according to Box-Behnken design of experiment, with additional runs. Pressure, temperature and flow rate were chosen as independent variables. Five well known empirical kinetic models and three mass-transfer kinetics models based on the Sovová's solution of SFE equations were successfully applied for kinetics modeling. The developed mass-transfer models exhibited better fit of experimental data, according to the calculated statistical tests (R2, SSE and AARD). The initial slope of the SFE curve was evaluated as an output variable in the ANN optimization. The obtained results suggested that it is advisable to lead SFE process at an increased pressure and CO2 flow rate with lower temperature and particle size values to reach a maximal initial slope.

Extraction of Peppermint Essential Oils and Lipophilic Compounds: Assessment of Process Kinetics and Environmental Impacts with Multiple Techniques.

Consumers are becoming more mindful of their well-being. Increasing awareness of the many beneficial properties of peppermint essential oil (EO) has significantly increased product sales in recent years. Hydrodistillation (HD), a proven conventional method, and a possible alternative in the form of microwave-assisted hydrodistillation (MWHD) have been used to isolate peppermint EO. Standard Soxhlet and alternatively supercritical fluid (SFE), microwave-assisted, and ultrasound-assisted extraction separated the lipid extracts. The distillations employed various power settings, and the EO yield varied from 0.15 to 0.80%. The estimated environmental impact in terms of electricity consumption and CO2 emissions suggested that MWHD is an energy efficient way to reduce CO2 emissions. Different extraction methods and solvent properties affected the lipid extract yield, which ranged from 2.55 to 5.36%. According to the corresponding values of statistical parameters, empiric mathematical models were successfully applied to model the kinetics of MWHD and SFE processes.

Pressurized-Liquid Extraction as an Efficient Method for Valorization of Thymus serpyllum Herbal Dust towards Sustainable Production of Antioxidants.

The aim of this study was to valorize Thymus serpyllum herbal dust, a particular fraction distinguished as an industrial waste from filter-tea production. Pressurized liquid extraction (PLE) was used with the aim of overcoming certain obstacles of conventional extraction techniques in terms of shortening extraction time, reducing solvent consumption and energy costs, using "green" solvents and obtaining high yield and quality products. In order to optimize PLE of T. serpyllum herbal dust, the preliminary screening of the independent variables in order to define the most influential parameters and their domain was done first. After the screening, the optimization study using the face-centered central composite experimental design (CCD) with response surface methodology (RSM) was implemented. Additionally, taking into account the high awareness of the positive influence of antioxidants on the human health and associating it with high content of polyphenolic compounds in various members of Lamiaceae family, PLE has proven to be a great approach for antioxidants recovery from T. serpyllum herbal dust.

Chemical composition and antimicrobial activity of Osage orange (Maclura pomifera) leaf extracts.

The main goal of this study was to establish the chemical profile of Osage orange (Maclura pomifera) leaf extracts, obtained by conventional maceration technique, and to examine its antimicrobial activity. The identification and quantification of the extract compounds were done using ultra-high-performance liquid chromatography, with a diode array detector coupled with triple-quadrupole mass spectrometer and gas chromatography-mass spectrometry techniques. Thirty-one polyphenolic compounds were detected and identified in the ethanolic extracts, whereby 5-O-caffeoylquinic acid was found to be the dominant compound. Among other compounds, pentacosane and palmitic acid were the most abundant compounds in the dichloromethane extract. The preliminary antimicrobial activity screening shows that Gram-positive bacteria tend to be more sensitive to the investigated extracts. The highest antimicrobial activity was determined against Enterococcus faecalis ATCC 19433 and Listeria monocytogenes ATCC 35152. From these results, Osage orange leaves can be considered as plant material with significant antimicrobial properties.

Antioxidant and enzyme-inhibitory activity of peppermint extracts and essential oils obtained by conventional and emerging extraction techniques.

Peppermint is widely used medicinal plant with distinguished bioactive potential, therefore, the aim of present work was to develop novel peppermint extracts with high activity by application of traditional and emerging separation techniques. Conventional hydrodistillation and microwave-assisted hydrodistillation (MWHD) were applied for recovery of essential oil (EO), while organic solvent extraction using Soxhlet apparatus, microwave-assisted and ultrasound-assisted process and supercritical fluid extraction (SFE) were applied for non-selective recovery of peppermint lipophilic extracts. Extracts were characterized in terms of terpenoids profile with special emphasis on content of major compounds (mentol, menthone, isomenthol and eucalyptol). Antioxidant activity (DPPH, ABTS, CUPRAC, FRAP, chelating and phosphomolybdenum assay) and enzyme-inhibitory assays (acetylcholinesterase, butyrylcholinesterase, tyrosinase, amylase and glucosidase inhibition) were used for screening of peppermint bioactivity. MWHD was recognized as alternative for traditional process in EO recovery, while SFE extracts were useful for green production of solvent-free peppermint extracts rich in terpenoids and other lipophilic bioactives.