Solid Extraction Research Articles

Phytochemical investigation, in-vitro antiplasmodial assessment and cytotoxic effect of ethanol extract of whole plant of Crotalaria arenaria (Benth)

Crotataria arenaria (Benth) is a native plant from Northern part of Nigeria which is employed as antimalarial herb in traditional medicine in the communities where it grows. The phytochemical composition, In-vitro antiplasmodial activity and in-vitro cytotoxic effect of the extract and fractions of the whole plant of Crotalaria arenaria were investigated. The mature and fresh whole plant of C. arenaria were collected, air dried and pulverized. The pulverized form of the plant were soaked in ethanol for two weeks and later decanted, filtered and concentrated using rotatory evaporator at 40oC and evaporated to dryness and labeled CRA-1. The dried ethanol solid extract (CRA-1) was patitioned/fractionated using water, chloroform, ethyl acetate, 18% aqueous methanol, n-hexane which afforded chloroform fraction (CRA-1-01), water fraction (CRA-1-02), ethyl acetate fraction (CRA-1-03) aqueous methanol fraction (CRA-1-04) and n-hexane (CRA - 1- 05) and they were dried and tested for their photochemicals and In-vitro antiplasmdial activity against Plasmodium falciparum strain (K1). The ethanol extract and its fractions were found to significantly inhibited/suppressed multi-drug resistant strain of P. falciparium (K1) in the range of 86.73% - 65.31% at varied concentrations of 5000 µg/ml, 2000 µg/ml, 1000 µg/ml and 500 µg/ml. The ethanol extract and its fractions showed the presence of tannins, saponins and alkaloids which could be responsible for the In-vitro antiplasmodial activity of the whole plant extract of C. arenaria and each of its fractions. Ethanol crude extracts of whole plant of Crotalaria arenaria and its fractions were investigated for cytotoxicity in Brine shrimp lethality Test (BSLT). Larvicidal activities were noticed with dosage concentration from 1000 µg/ml down to 10 µg/ml of the plant extract and all its fractions. The relative cytotoxic effects of extract and fractions obtained from whole plant of Crotalaria arenaria were found to be dose-dependent because higher dosage brought about an increase in mortality of Artemia salina Leach. Sea salty water of the crude ethanol extract and its fractions served as the negative control. The chloroform fraction was observed to be most cytotoxic killing 30% of brine shrimp larvae at lowest concentration of 10 µg/ml with average percentage lethality of 46.67%. Aqueous methanol and ethanol crude extract appears to show similar and closely related activities against brine shrimp larvae at highest concentration of 1000 µg/ml. The ethanol crude extract and aqueous methanol fractions are toxic at higher dosage as they were found to induce significant mortality effect (In-vitro) against Artemia salina Leach particularly at concentration of 1000 µg/ml and therefore not safe for oral consumption especially at higher uncontrolled doses but at relatively low/moderate doses. The findings in this present study demonstrated that the extract of C. arenaria (whole plant) and fractions have significant in vitro antiplasmodial activity and this has justified the traditional use of the whole plant extract of Crotaria arenaria in the folklore medicine to cure malaria related illness. The results obtained in this study may serve as key data for utilization of Crotalaria arenaria in the development of bioactive agents which could be used as antimalarial, anticancer, pesticidal, insecticidal and anti-proliferation agents. The study recommended in-vivo antiplasmodial assay of the extract of the whole plant of Crotalaria arenaria to further substantiate the findings of this present study.

Efficient alcoholysis of total saponins in D. zingiberensis to diosgenin using ionic liquid-grafted MOF superacids

Diosgenin is an indispensable intermediate in the production of various steroid drugs. Conventional hydrolysis of sulfuric acid produces large amounts of acidic wastewater and has always faced stringent restrictions from environmental requirements. Here, UiO-66-NH2 and its derivative of UiO-66-NH2-AT (AT = 3-amino-1,2,4-triazole) were synthesized, and these two compounds were further grafted with high-concentration CF3SO3H molecules to obtain the MOF-based solid superacids, namely UiO-66-NH2-[SO3CF3] and UiO-66-NH2-AT-[SO3CF3], respectively. They have been applied to the alcoholysis of total saponins to extract diosgenin, and the alcoholysis conditions, including the solid acid dosage, extraction temperature and extraction time, have been optimized by single-factor experiments. Subsequently, the alcoholysis conditions of UiO-66-NH2-AT-[SO3CF3] with more prominent catalytic performance and cycle stability were further optimized by the response surface method, and under the optimum conditions, the diosgenin yield reached 20.8 %, which was close to the predicted value of 21.3 % and was superior to the conventional hydrolysis of sulfuric acid and our previously reported solid acids. Additionally, the alcoholysis pathways and alcoholysis mechanism of the total saponins catalyzed by UiO-66-NH2-AT-[SO3CF3] have been proposed by the analysis of high-resolution electrospray mass spectrometry.

Isolation and Characterization of Indigenous Bacteria with Purifying Potential in Solid Palm Oil Extraction Sludge Generated by SOCAPALM-Mbambou

The oil palm industry contributes significantly to the economic development of producing countries such as Cameroon. Unfortunately, the exploitation of palm oil constitutes a source of environmental pollution due to the production of enormous quantities of waste during its extraction process, including solid sludge generating greenhouse gases which contribute to global warming climatic. All this leads to the search for alternatives which consists of isolating and characterizing indigenous bacteria with biodegradation capacities in sludge from palm oil extraction. The pH and bacterial counts were determined by the potentiometric method and the decimal dilution technique, respectively. The isolated bacteria were identified by their cultural, cellular and biochemical characteristics. In addition, the identification of Gram- bacteria was further explored by the API 20 E gallery. The palm oil biodegradability test was carried out on M2 medium supplemented with 2% palm oil. The solid sludge biodegradability test was carried out on liquid MSM medium supplemented with 4% sludge stock solution. The results showed that the sludge sample had a slightly alkaline pH of 7.3. A bacterial load of around 10<sup>9</sup> CFU/g of soil was counted. Thirty-one bacterial strains were isolated and purified, including 12 <i>Bacillus sp</i>, 10 <i>Pseudomonas sp</i>, 8 <i>Proteus mirabilis</i> and 1 <i>Klebsiella pneumoniae</i>. All isolates tested for their ability to degrade palm oil or solid sludge grew in culture media with palm oil or solid sludge as the sole source of carbon and energy but with a difference in load. Thus, isolates BI2, BI5, BI31, BI10 and BI 9 showed the highest degradation capacities. These isolates could be used to constitute consortia of microorganisms that can be used in the treatment of waste generated by palm oil extraction.

Multigene phylogeny, bioactive properties, enzymatic and dye decolorization potential of selected marine fungi from brown algae and sponges of Mauritius

Marine fungi represent an important proportion of the microbial diversity in the oceans. They are attractive candidates for biotechnological purposes and industrial applications. Despite an increasing interest in mycology, marine fungi associated with sponges and algae have been poorly studied in Mauritius. The objectives of this study were to: 1) use multigene phylogenetic analyses to identify isolated marine fungi; 2) determine the differences in the antimicrobial and antioxidant properties of the fungal extracts; and 3) assess their enzyme activities and dye decolorization potential. Five fungal isolates viz Aspergillus chevalieri, Aspergillus iizukae, Aspergillus ochraceus, Exserohilum rostratum and Biatriospora sp. were identified based on phylogenetic analyses. There was no significant difference in the antimicrobial properties of the liquid and solid media extracts unlike the antioxidant properties (p < 0.05). The solid media extract of Aspergillus chevalieri (F2-SF) had a minimum inhibitory concentration of 0.156 mg/ml against Staphylococcus aureus while Aspergillus ochraceus (F25-SF) had a minimum inhibitory concentration of 0.313 and 2.5 mg/ml against Enterococcus faecalis and Salmonella typhi. The solid media extract of Biatriospora sp. (F34-SF) had a minimum inhibitory concentration of 0.195 and 1.563 mg/ml against Bacillus cereus, Escherichia coli and Enterobacter cloacae. An IC50 of 78.92 ± 4.71 μg/ml in the 2,2-Diphenyl-1-picrylhydrazyl (DPPH) scavenging assay, ferric reducing antioxidant power (FRAP) value of 11.17 ± 0.20 mM Fe2+/g dry weight extract (DWE) and total phenolic content 360.35 ± 10.31 mg GAE/g DWE was obtained with the solid media extract of Aspergillus chevalieri (F2-SF). Aspergillus ochraceus (F25-SF) and Biatriospora sp. (F34-SF) solid media extracts showed lower IC50 values in the DPPH assay and higher total phenolic content as compared to the liquid media extracts. Aspergillus chevalieri was a good producer of the enzymes DNAse and lipase and had maximum percentage dye decolorization of 79.40 ± 17.72% on Congo red. An enzymatic index ≥ 2 was found for the DNAse and lipase and the maximum percentage dye decolorization of 87.18 ± 3.80% was observed with Aspergillus ochraceus on Methylene blue. Regarding Biatriospora sp., it was a moderate producer of the three enzymes amylase, DNAse and protease and had a maximum dye decolorization potential of 56.29 ± 6.51% on Crystal violet. This study demonstrates that Mauritian marine fungi possess good bioactive properties, enzymatic and dye decolorization potentials, that can potentially be considered for use in pharmaceutical and industrial applications.

Determination of the Thermal Stability of Impregnated Type Solid Extractant Based on Dibenzo-21-crown-7 and Organic Matrix MN-200

Determination of the Thermal Stability of Impregnated Type Solid Extractant Based on Dibenzo-21-crown-7 and Organic Matrix MN-200

A novel headspace solid-phase microextraction arrow method employing comprehensive two-dimensional gas chromatography–mass spectrometry combined with chemometric tools for the investigation of wine aging

BackgroundOmics is used as an analytical tool to investigate wine authenticity issues. Aging authentication ensures that the wine has undergone the necessary maturation and developed its desired organoleptic characteristics. Considering that aged wines constitute valuable commodities, the development of advanced omics techniques that guarantee aging authenticity and prevent fraud is essential. ResultsΑ solid phase microextraction Arrow method combined with comprehensive two-dimensional gas chromatography-mass spectrometry was developed to identify volatiles in red wines and investigate how aging affects their volatile fingerprint. The method was optimized by examining the critical parameters that affect the solid phase microextraction Arrow extraction (stirring rate, extraction time) process. Under optimized conditions, extraction took place within 45 min under stirring at 1000 rpm. In all, 24 monovarietal red wine samples belonging to the Xinomavro variety from Naoussa (Imathia regional unit of Macedonia, Greece) produced during four different vintage years (1998, 2005, 2008 and 2015) were analyzed. Overall, 237 volatile compounds were tentatively identified and were treated with chemometric tools. Four major groups, one for each vintage year were revealed using the Hierarchical Clustering Analysis. The first two Principal Components of Principal Component Analysis explained 86.1% of the total variance, showing appropriate grouping of the wine samples produced in the same crop year. A two-way orthogonal partial least square – discriminant analysis model was developed and successfully classified all the samples to the proper class according to the vintage age, establishing 17 volatile markers as the most important features responsible for the classification, with an explained total variance of 88.5%. The developed prediction model was validated and the analyzed samples were classified with 100% accuracy according to the vintage age, based on their volatile fingerprint. SignificanceThe developed methodology in combination with chemometric techniques allows to trace back and confirm the vintage year, and is proposed as a novel authenticity tool which opens completely new and hitherto unexplored possibilities for wine authenticity testing and confirmation.

Cucurbit[7]uril-mediated matrix solid phase dispersion extraction strategy combined capillary electrophoresis for detection of biogenic amines in foods

Biogenic amines (BAs) are the vital indicators of food freshness, and monitoring the change of BAs content is quite essential for food safety. Herein, we developed a matrix solid phase dispersion (MSPD) extraction technology based on cucurbit[7]uril (Q[7]) to extract BAs from pork and shrimp. Then, the extracted BAs were analyzed by capillary electrophoresis (CE) with low sample consumption and high analytical efficiency. The factors affecting MSPD extraction were optimized by Plackett-Burman and the Box-Behnken design (BBD). The limits of detection (LODs) were ranging from 0.003 to 0.019 mg kg−1, the recoveries of spiked samples were 80.15 %–110.3 %. The satisfactory accuracy and precision were attributed to the host–guest interaction between Q[7] and BAs. Furthermore, the freshness of pork and shrimp was evaluated by simultaneous determination of four BAs. For its wide linear range, high sensitivity, and cost-effectiveness, the proposed Q[7] mediated MSPD-CE-UV provides meaningful potential prospects in the rapid monitor of food freshness and safety.

Optimizing callus formation in the endangered medicinal tree Hydnocarpus macrocarpa using phytohormone

Hydnocarpus macrocarpa (Flacourtiaceae) is one of the endemic and endangered medicinal tree, was selected to investigate the influence of plant growth regulators on callus formation. H. macrocarpa is majorly distributed at low and medium elevations of the Southern Western Ghats. The seeds of this plant are used for the treatment of ulcers, biliousness, leprosy and epilepsy. An experiment was carried out with two different methods. In the first method Murashige and Skoog (MS) medium supplemented with cytokinin alone or combined with auxin (2–4-Dichlorophenoxy acetic acid; Naphthalene acetic acid; Indole acetic acid; Indole butyric acid and Gibberellic acid) at different concentrations (1, 2, 3, 4 and 5 µM) were used; in the seond method, MS medium supplemented with coconut endosperm (Solid and liquid) extract (1, 2, 3, 4 and 5 %) with Aloe vera jelly extract at different concentrations (1, 2, 3, 4 and 5 %) in combination and separately were used. Among the different treatments, good callus proliferation was obtained using MS medium supplemented with Benzylaminopurine and in combination with Naphthalene acetic acid and 2–4-Dichlorophenoxyacetic acid (3 µM and 4 µM). But the best callus proliferation, shoot tip proliferation; auxiliary root and shoot formation were observed in MS medium supplemented with Aloe vera jelly extract in combination with coconut endosperm extract. The natural growth regulators supplemented with the media gave a positive response for plant growth. The results showed that the natural growth regulators, such as coconut endosperm and Aloe vera jelly extracts were found to be more efficient than the synthetic growth regulators (auxin and cytokinin). The presence of Indole acetic acid and Indole butyric acid in both Aloe vera jelly extracts and coconut endosperm were confirmed by High performance liquid chromatography and Fourier transform infrared spectroscopy analysis.

Solid Phase Oligo-DNA Extraction from Complex Medium Using an Aminated Graphene/Nitrocellulose Membrane Hybrid.

A hybrid material, consisting of commercially available nitrocellulose (NC) membrane non-covalently modified with amino-polyethylene glycol functionalized reduced graphene oxide (NH2-PEG-rGO) nanoparticles, was successfully synthesized for oligonucleotide extraction. Fourier Transform Infrared Spectroscopy (FTIR) confirmed the modification of the NC membrane, revealing characteristic peaks of both compounds, i.e., NC and NH2-PEG-rGO. Scanning Electron Microscopy (SEM) exhibited morphological changes in the NC/NH2-PEG-rGO hybrid membrane, marked by the introduction of NH2-PEG-rGO particles, resulting in a distinctly smothered surface compared to the porous surface of the NC control membrane. Wettability assays revealed hydrophobic behavior for the NC/NH2-PEG-rGO hybrid membrane, with a water contact angle exceeding 90°, contrasting with the hydrophilic behavior characterized by a 16.7° contact angle in the NC membrane. The performance of the NC/NH2-PEG-rGO hybrid membrane was evaluated for the extraction of ssDNA with fewer than 50 nucleotides from solutions containing various ionic species (MnCl2, MgCl2, and MnCl2/MgCl2). The NC/NH2-PEG-rGO hybrid membrane exhibited optimal performance when incubated in MgCl2, presenting the highest fluorescence emission at 525 relative fluorescence units (r.f.u.). This corresponds to the extraction of approximately 610 pg (≈13%) of the total oligo-DNA, underscoring the efficacy of the pristine material, which extracts 286 pg (≈6%) of oligo-DNA in complex solutions.

Preparation of magnetic amphiphilic resin microspheres via the one-step polymerization method and extraction of four glucocorticoids for HPLC–MS analysis

Amphiphilic materials can be used for sample preparation of chromatography or mass spectrometry. Amphiphilic materials with magnetic properties in combination with magnetic suction devices allow for automated sample preparation. However, conventional synthesis methods are cumbersome and not suitable for the mass production of the material. In this study, a micro-suspension polymerization method was developed to synthesize magnetic amphiphilic resin microspheres (MARMs), providing new ideas for the preparation of amphiphilic microspheres. MARMs with particle sizes ranging from 3 to 6 μm were successfully prepared, with BET surface area up to 653.2 m2/g. A magnetic solid-phase extraction method based on MARM-5 was developed for the extraction of four glucocorticoids including Cortisone, Hydrocortisone, Cortodoxone, and Corticosterone. This method had a very short adsorption time of 0.5 min and a total extraction time of only 13 min. The limit of detection for the four glucocorticoids ranged from 0.22 to 0.82 ng/L. There was a good linear relationship between sample concentration and peak area in the range of 25∼500 ng/L. Relative recovery of 98 %∼108 % and internal standard normalized matrix effect factors of 95∼114 % were obtained, and the relative standard deviation was between 2.3 % and 6.3 %. The MARMs would be used as excellent solid extraction material for glucocorticoids.

Superior high-efficiency and high-throughput volatile flavor extraction of Japanese fermented seasonings by solvent-assisted stir bar solid extraction with reverse extraction

Fermented seasonings have pleasant flavors that stimulate our appetite. Their flavoring properties change depending on factors such as their materials and fermented conditions. Therefore, a comparative analysis of their flavor is important when evaluating their quality. However, seasonings contain high levels of various matrices such as sugars, proteins, lipids, and ethanol, making it difficult to extract aroma compounds efficiently from them. In this study, we verified a high-efficient and high-throughput volatile flavor analysis of fermented seasonings by solvent-assisted stir bar solid extraction (SA-SBSE) with reverse extraction. We applied SA-SBSE to Japanese fermented seasonings, soy sauce, miso (fermented beans), and mirin (sweet rice wine) and compared their profiles with those from other common extraction methods, headspace gas-solid-phase microextraction (HS-SPME), liquid extraction with solvent-assisted flavor evaporation (LE-SAFE), and conventional SBSE (C-SBSE). The aroma properties and profiles of extracts from SA-SBSE were close to those of the original sample, being similar to that of LE-SAFE. In addition, potent aroma compounds in each sample were extracted by SA-SBSE and LE-SAFE, which were far superior to those by C-SBSE. For quantification, SA-SBSE extracts showed a good standard curve by the standard addition method. We could quantify maltol, one of the most common potent aroma compounds in all samples, for various commercial samples by such high-throughput analysis.

Combination of a Deep Eutectic Solvent and Macroporous Resin for Green Recovery of Iridoids, Chlorogenic Acid, and Flavonoids from Eucommia ulmoides Leaves.

To increase the effectiveness of using typical biomass waste as a resource, iridoids, chlorogenic acid, and flavonoids from the waste biomass of Eucommia ulmoides leaves (EULs) were extracted by deep eutectic solvents (DESs) in conjunction with macroporous resin. To optimize the extract conditions, the experiment of response surface was employed with the single-factor of DES composition molar ratio, liquid-solid ratio, water percentage, extraction temperature, and extraction time. The findings demonstrated that the theoretical simulated extraction yield of chlorogenic acid (CGA), geniposidic acid (GPA), aucubin (AU), geniposide (GP), rutin (RU), and isoquercetin (IQU) were 42.8, 137.2, 156.7, 5.4, 13.5, and 12.8 mg/g, respectively, under optimal conditions (hydrogen bond donor-hydrogen bond acceptor molar ratio of 1.96, liquid-solid ratio of 28.89 mL/g, water percentage of 38.44%, temperature of 317.36 K, and time of 55.59 min). Then, 12 resins were evaluated for their adsorption and desorption capabilities for the target components, and the HPD950 resin was found to operate at its optimum. Additionally, the HPD950 resin demonstrated significant sustainability and considerable potential in the recyclability test. Finally, the hypoglycemic in vitro, hypolipidemic in vitro, immunomodulatory, and anti-inflammatory effects of EUL extract were evaluated, and the correlation analysis of six active components with biological activity and physicochemical characteristics of DESs by heatmap were discussed. The findings of this study can offer a theoretical foundation for the extraction of valuable components by DESs from waste biomass, as well as specific utility benefits for the creation and development of natural products.

Subcritical water extraction of red cabbage regarding cholinesterase and tyrosinase inhibitory activity

Pressurized high-temperature processing of water where polarity can be regulated has been an advanced extraction technology considering sustainable management and efficient use of natural resources. In this study, subcritical water extraction of red cabbage and its enzyme inhibitory potential were investigated using response surface methodology. Spectrophotometric quantification was utilized for total phenol, flavonoid, and anthocyanin contents, while dominant anthocyanin molecules were identified with UPLC-DAD, ESI-MS/MS. The 200 bar-120°C-30 min-30 solvent:solid ratio extract was determined with the highest total anthocyanin content (2.33 mg Cya3GluE/g), where cyanidin-3-sophoroside-5-glucoside, cyanidin-3-(sinapoyl)-sophoroside-5-glucoside, and cyanidin-3-(sinapoyl)(sinapoyl)-sophoroside-5-glucoside were identified as the dominant anthocyanins (1.15 mg Cya3GluE/g). IC50 values for acetylcholinesterase, butyrylcholinesterase, and tyrosinase inhibitory activities were found to be 0.058 mg/ml, 0.215 mg/ml, and 0.86 mg/ml, respectively (tenfold superior to solvent extract). Despite the well-known high-temperature lability of phenolic compounds, subcritical water proved to be useful as a more selective system for extracting red cabbage bioactives with enzyme inhibitory activity when appropriate process conditions could be determined.

Phosphonate functionalized magnetic mesoporous silica for rare earth element recovery from citrate assisted solid waste extracts

The growing high demand of rare earth elements (REEs) has prompted extensive research on REE recovery from waste streams. This study reports the synthesis and evaluation of phosphonate-functionalized magnetic mesoporous silica (MMS-PP) for REE recovery from the acidic extracts of solid wastes. MMS-PP was synthesized using surfactant template and post-synthesis methods, and tested using simulated and real extraction solutions from citrate-assisted REE extracts from municipal solid waste incineration (MSWI) ash. The organic-inorganic hybrid MMS-PP was evaluated for La recovery from 50 mM simulated citrate extract, with the adsorption capacity of 13.5 mg/g compared to ∼2.5 mg/g for non-functionalized MMS. The MMS-PP material exhibited fast adsorption within 10 min, good La selectivity against competing Na+ and Ca2+, moderate selectivity against Al3+ and Fe3+, high recyclability over multiple adsorption-desorption cycles, and equivalent efficiency for La, Ce, Nd, and Y recovery. The MMS-PP material also demonstrated 70–95% REE recovery from real citrate extracts of MSWI ash, and the spent MMS-PP material can be regenerated and reused for multiple cycles. Functionalized mesoporous materials in combination with organic-ligand assisted extraction can potentially provide a green, effective, and tunable solid-liquid separation platform for REE recovery from complex solid waste streams.

Simultaneous production of dry solid biomass and liquid extract from Sorghum bicolor using liquefied ammonia

Energy-consuming processes should be avoided while separating biomass components. This study investigated the dewatering and extraction of components from Sorghum bicolor silage using liquefied NH3 (NH3(l)). Using a plug-flow-type reactor, NH3(l) was passed through the specimen at 20 °C and 0.85 MPa. When the NH3/wet sample weight was 4.7, a 31.0 wt% dry ammonia-treated sample (AT) was obtained as an extract, achieving a 96.5 wt% dewatering ratio. Glucose, xylose, and an acid-insoluble fraction were retained in the AT, whereas lactic and acetic acids were separated as an extract. Crystalline cellulose was transformed, and the increase in glucose and xylose yields from the enzymatic hydrolysis of the AT was similar levels to those from sulfuric acid hydrolysis. Therefore, NH3(l) treatment can dewater S. bicolor silage without severe pretreatment. In addition, it can be used in biofuel and chemical production using enzymatically degradable ATs from which organic acids are separated as extracts.

Chemical profiling and biological activity assessment of volatile and non-volatile compounds in Rosmarinus officinalis residues

Rosmarinus officinalis L. is a Mediterranean medicinal and aromatic plant, widely used in several industries. The present study aimed to characterize the chemical composition of volatile compounds, encompassing essential oils (EO): hydrosol extract (HE): and water residue extract (WRE1). Additionally, the investigation focused on non-volatile components, including powder phenolic extract (PPE): water residue extract (WRE2): and solid residue extract (SRE): while also assessing their antioxidant and antibacterial activities. The chemical compositions of volatile components were determined by using a Gas Chromatograph equipped with a Mass Spectrometer (GC/MS): while polyphenol extracts were analyzed using Ultra-High-Performance Liquid Chromatograph equipped with a photodiode array detection Mass Spectrometer (UHPLC-DAD-ESI/MS). The antioxidant activity was determined by 1,1-diphenyl-2-picrylhydrazyl free radical scavenging (DPPH) and ferric reducing antioxidant power (FRAP): while the antibacterial effect was evaluated against four pathogenic bacterial strains using disc diffusion and broth microdilution methods. The GC/MS analysis showed that R. officinalis EO was dominated by 1,8-cineole (47.70%) and α-pinene (15.50%). 1,8-cineole (56.67%) and camphor (26.27%) were found as the predominant constituents of HE, while volatile components of WRE1 were mainly dominated by camphor (10.11%). The UHPLC-DAD-ESI/MS analysis revealed the existence of a plethora of polyphenolic components. In PPE and SRE, the predominating compounds were carnosic acid and carnosol, respectively. Rosmarinic acid was the main constituent in WRE2. The results of DPPH free radical scavenging and FRAP activities showed that PPE exhibited strong antioxidant activity, followed by SRE and WRE2. EO and HE showed moderate antioxidant activity, while volatile components of WRE1 exhibited the lowest antioxidant effect. Regarding the antibacterial activity, PPE and SRE indicated the highest effect against the pathogenic bacteria, while WRE1 volatile components had the weakest antibacterial activity. The conducted study showed that material plant left after hydrodistillation of R. officinalis may be used as a new source of bioactive volatile and polyphenolic components with valuable pharmacological activities.

ПРИМЕНЕНИЕ МЕТОДА ПРОГНОЗИРОВАНИЯ СОСТОЯНИЯ МАССИВА В СЛОЖНЫХ ГОРНО-ГЕОЛОГИЧЕСКИХ УСЛОВИЯХ

The existing hydrogeological, instrumental and analytical methods of determining the location of the upper boundary of the zone of technogenic water-conducting cracks do not allow to predict its change in time in complex mining and geological conditions and taking into account the high rates of solid minerals extraction. Their application involves high risks of technogenic accidents. The developed method of predicting the condition of the rock massif on the basis of regularities of distribution of deformations in the developed massif on the example of solid minerals deposit is considered in the paper. The regularities obtained from the results of processing of field measurements are adapted and make it possible to forecast the development of geomechanical parameters taking into account the approved plans of mining operations, which provides the safety of the mine.

Volatile Metabolite Profiles of Robusta Green Bean Coffee From Different Geographical Origins in West Java and Their Correlation With Temperature, Rainfall, and Altitudes Using SPME GC‐MS–Based Metabolomics

The chemical composition, including volatile metabolites of green coffee beans, is influenced by geographic origin. The aim of this study was to reveal the volatile metabolite profile of a single variety of Robusta green bean coffee from five major plantation regions in West Java and to correlate these profiles with temperature, rainfall, and altitude. By using solid phase micro extractions and gas chromatography‐mass spectrometry, 143 different volatile compounds were detected, with aromatic hydrocarbon, alcohols, monoterpene, pyrazines, sesquiterpenes, carboxylic acids, and terpene the most dominant. Principal component analysis (PCA) indicated 64.3% variability, showing that the metabolite profile of Robusta green coffee from the Bogor region was distinctly different from those in Ciamis, Kuningan, Sumedang, and Tasikmalaya, which were more similar to each other. Metabolites such as benzaldehyde, isovaleric acid, toluene, diisobutyl succinate, 1‐heptene, 4‐dodecene, caffeine, acetic acid, and methyl benzoate were identified as key discriminants, with a VIP score greater than 1.5. Temperature increases were linked to higher levels of isovaleric acid, diisobutyl succinate, 4‐dodecene, toluene, and acetic acid, while other discriminant metabolites declined. Increased rainfall was associated with higher levels of benzaldehyde, 1‐heptene, caffeine, and methyl benzoate, but lower levels of the other discriminants. Altitude had a positive correlation with methyl benzoate and 1‐heptene, and a negative correlation with isovaleric acid and 4‐dodecene, with weaker correlations for other compounds. In summary, Robusta green coffee beans from different regions of West Java can be distinguished by their volatile metabolites. Bogor green coffee beans had higher levels of benzaldehyde, 1‐heptene, caffeine, and methyl benzoate, Kuningan beans had more diisobutyl succinate and 4‐dodecene, Ciamis beans had higher levels of isovaleric acid, diisobutyl succinate, and 4‐dodecene, while Sumedang and Tasikmalaya beans were similar, with higher levels of isovaleric acid, diisobutyl succinate, 4‐dodecene, toluene, and acetic acid. This difference is related to the climatic factors of temperature and rainfall, as well as the altitude at which Robusta coffee is grown.

An Effective Sol-Gel-Functionalized Polyurethane Foams Solid Platform Packed Minicolumns for Complete Extraction of Chromium (VI) from Water: Kinetic, Sorption Isotherms, Thermodynamic Study, and Analytical Utility.

In the modern era, sol-gel plays a key role in the progress of a new generation of dispersive solid-phase microextractors (d-µ SPMEs) for the removal of organic and inorganic pollutants in complex matrices. Thus, the current study reports the use of sol-gel-functionalized polyurethane foams (PUFs) as a novel solid platform for complete extraction of chromium (VI) species from aqueous media. The planned protocol was based upon the complete extraction of the formed binary complex ion associates between the protonated ether and/or urethane groups of PUFs and chlorochromate anion [CrO3Cl]- aq in aqueous HCl (≥1M) medium in addition to H-bonding and the electrostatic π-π interaction that resulted between the CrO3Cl- and the silanol group (Si/ZrO2, Si-O-Zr) and siloxane (Si-O-Si) groups of the sol-gel. The impact of the analytical parameters (solution pH, natural mineral acids, shaking time, temperature, and chromium (VI) concentrations) was critically studied. At the optimal conditions, the uptake capacity of the established extractor (9.9 mg·g-1) was in agreement with the Langmuir adsorption capacity (12.08 mg·g-1) of the monolayer. The sorption data fitted well with the pseudo first-order kinetic model (R 2 = 0.9961) with an overall rate constant (k 1) of 0.081 min-1 and an equilibrium capacity (q e ) of 8.6 mg·g-1, which is in a good agreement with the experimental value (9.9 mg·g-1). The sorption of the oxyion [CrO3Cl]- aq onto the solid sorbent is an endothermic and spontaneous process as reflected from the values of ΔH (6.99 kJ·mol-1) and ΔG (-8.14 kJ·mol-1 at 293 K), respectively. The ΔS value (15.13 kJ·mol-1·K-1) reflects that the [CrO3Cl]- aq retention onto the sol-gel-treated PUFs sorbent proceeded in a more unplanned fashion. Sol-gel-treated PUFs sorbent-packed minicolumns were successfully used for the complete removal of trace levels of chromium (VI) species from water samples. Sorbed chromium (VI) species were recovered with NaOH (0.5 M) and analysed by spectrophotometry, which supports the utility of the sol-gel-treated PUFs as a low-cost solid extractor for water treatment.

The Variation Effect of Solvents on the Physicochemical Properties Baobab (Ophelussitularius) Seeds Oil

It is remarkable to notice that Baobab seeds are normally discarded in Sudan, without knowing the great wealth hidden. The present study was conducted to determine physicochemical properties of Baobab (Ophelussitularis) seeds oil and select proper solvent for oil extraction from seeds which contain approximately 22-45%, used n-hexane and ethanol as solvents, leaching was done by solid extraction method. Physicochemical properties of the Baobab seeds oil were evaluated by standard and established methods. Oils and solvents were separated using rotary evaporator, recovery solvent were 91.2% and 75% for n-hexane and ethanol respectively. The obtained Baobab oils color were golden yellow (reddish yellow) not effected by type of solvent, it showed resistance to change in color, results showed the maximum Baobab oil yields were 16% and 13.5 % for n-hexane and ethanol respectively. Crude protein CP was found to be13.475 g/100 g, oil content was 13.26 g/, Saponification value SV 338.4925 g and 406.725 g/100 g for Baobab oil extracted with n-hexane and ethanol respectively. Results were obtained for ash content, crude fiber, acid value, FFA and rheological properties. Physicochemical properties indicated that n-hexane was more suitable to extract Baobab oil more than ethanol and recover easy. The difference was clearly visible in PV, AV and µ, while n-hexane yields pure oil more than ethanol. All those results detected that seeds of Baobab are beneficial if they extracted using n-hexane. It is recommended to conduct additional research on this issue and insert other solvents to select the best solvent and study the effect of different solvents on the properties of resulting oil.