Optimized Extraction Method Research Articles

Biopesticidal Potential of Indigenous Plant Extracts against Rice Weevil in Stored Wheat

Stored products are significantly affected by certain well-known stored grain pests, with Sitophilus oryzae L. (Coleoptera: Curculionidae) being one of the most destructive pests of stored products. It is a primary pest that causes substantial quantitative and qualitative losses. The present study was conducted to investigate the insecticidal efficacy of different plant extracts from four commonly grown plants in Pakistan: ginger (Zingiber officinale), neem (Azadirachta indica), clove (Syzygium aromaticum), and tobacco (Nicotiana tabacum) against S. oryzae infesting stored wheat. Crude extracts from these plants were applied to stored wheat at various dose rates (20, 40, 60, 80 mg). Adults of S. oryzae were introduced to the treated wheat and observed for mortality, repellency, and grain damage. The results of the study indicated that the maximum mortality of S. oryzae (99.17%) was recorded due to the application of crude extract of Z. officinale, while the minimum mortality of S. oryzae (67.50%) was recorded due to the crude extract of N. tabacum at an 80 mg dose rate after a 10-day exposure interval. The maximum grain damage due to S. oryzae (0.19%) was observed in N. tabacum treated crude extract at an 80 mg dose rate, while the minimum grain damage due to S. oryzae (0.04%) was observed in Z. officinale treated crude extract at an 80 mg dose rate. Z. officinale also exhibited the maximum repellent effect on S. oryzae (95.77%). This study concluded that Z. officinale emerged as a potent, readily available biopesticide against S. oryzae, surpassing current alternatives with near-eradication efficacy, minimal grain damage, and a proactive repellent effect, paving the way for sustainable and eco-friendly pest management. Further research is needed to optimize extraction methods, dosage recommendations, and assess long-term effects on grain quality and storage stability.

Seeking Optimal Extraction Method for Augmenting Hibiscus sabdariffa Bioactive Compounds and Antioxidant Activity

The dried flowers of Hibiscus sabdariffa (HS), available worldwide, have various applications in both non-medicinal and medicinal fields. The growing global interest in the health benefits of HS is linked to its potential prevention or management of non-communicable diseases. The aim of this research was to find the optimal extraction method that ensures the maximum yield of multiple beneficial bioactive components, such as polyphenols, anthocyanins, vitamin C, β-carotene, antioxidant activity, free radical scavenging activity DPPH and ferric reducing antioxidant power (FRAP). To this end, stirring, pulsed electric field, and ultrasound-assisted extraction were evaluated, either alone or in combination. Under optimized extraction conditions, the obtained extract exhibited an elevated total polyphenol content (37.82 mg of gallic acid equivalents/g dry weight (dw)), total anthocyanin content (610.42 μg of cyanidin equivalents/g dw), total carotenoids content (921.84 μg of β-carotene equivalents/g dw), and ascorbic acid content (507.44 mg/100 g dw). Remarkably, the extracts exhibited strong antioxidant properties (487.51 μmol of ascorbic acid equivalents (AAE)/g dw and 243.42 μmol AAE/g dw as evidenced by FRAP and DPPH assays, respectively). This research advances the parameters that should be employed to produce the optimal and nutritionally enhanced HS flower extracts, that can be used in the commercial sector.

Подбор и оптимизация методов экстракции ДНК из листьев гледичии трехколючковой (Gleditsia triacanthos L.)

Abstract. Currently, molecular genetic methods using DNA markers are increasingly used in studies of polymorphism of various populations of woody and shrubby plants. The purpose of this work was the evaluation and selection of protocols for the isolation and purification of DNA from the leaves of Gleditsia triacanthos L. for further studies using DNA labeling. Methods. Four protocols were used to isolate DNA from the leaf blade of Gleditsia triacanthos L. Anionic detergent sodium dodecyl sulfate was used in three isolation protocols for cell lysis, potassium acetate was used for purification from polysaccharides and proteins. In the fourth protocol, a cationic surfactant cetyltrimethyl ammonium bromide was used for cell lysis, the extract was purified with a mixture of chloroform-isoamyl alcohol (24 : 1). Precipitation of the isolated DNA was carried out with isopropanol. The quality of the isolated DNA was evaluated by spectrophotometry, horizontal electrophoresis and Real-time PCR with two types of primers. Results. Optimal conditions for DNA extraction from samples of Gleditsia triacanthos L. containing a large number of metabolites affecting the quality of the isolated extract were selected. By electrophoresis, it was found that both the isolation protocol with sodium dodecyl sulfate and the isolation protocol with cetyltrimethyl ammonium bromide make it possible to obtain a sufficient amount of DNA. The most purified DNA was obtained by the third protocol using sodium dodecyl sulfate and dithiotreitol and by the fourth protocol using cetyltrimethylammonium bromide. The results of PCR of the obtained samples with ITS and psbI-psbK primers indicate that a sufficient amount of product has been obtained and the reproducibility of ISSR markers. The scientific novelty of the work consists in choosing the optimal method of DNA extraction from the leaves of Gleditsia triacanthos L., which is a complex object containing a large number of potential PCR inhibitors. The protocol with sodium dodecyl sulfate and dithiotreitol made it possible to obtain DNA in the right amount and of acceptable quality.

Promising growth inhibitory potential of extracted natural silk sericin biopolymer against DEN‐induced liver tumor in male mice

AbstractSilk sericin (SS), a protein biopolymer, is gaining an increasing attention in a variety of biomedical applications. Our objective was to identify the optimal extraction method yielding the highest silk protein content, to assess its chemical elemental composition, to characterize it, and to compare its conformation by X‐ray diffraction and Fourier‐transform infrared versus that of the commercial one. Herein, alkali and high temperature is the perfect approach. This study aimed further to test whether extracted SS could attenuate the adverse hepatotoxic effects induced by diethylnitrosamine (DEN) in mice. Animals were injected intraperitoneally once weekly for four consecutive weeks with physiological saline (0.9% NaCl), DEN (25 mg/kg), SS (1 g/kg) 90 min prior to DEN injection, melatonin (10 mg/kg) followed within 1 h with the administration of SS and 30 min later with DEN. The results confirmed the hepatotoxicity of DEN manifested by an increase in liver enzymes' activity, and pathological changes in the liver tissue. The combined use of SS and/or melatonin with DEN returned most of the parameters to values similar to the controls. Briefly, chemically characterized SS seems a valuable extract for further consideration as anti‐carcinogenic agent. It has the potential to upgrade liver cancer chemotherapeutic agents.

Deep eutectic solvent (DES)-assisted extraction of pectin from Ficus carica Linn. peel: optimization, partial structure characterization, functional and antioxidant activities.

The pectin from Ficus carica Linn. (fig) peels is a valuable and recyclable constituent that may bring huge economic benefits. To maximize the utilization of this resource, deep eutectic solvent (DES)-assisted extraction was applied to extract pectin from fig peels, and the extraction process was optimized with response surface methodology. When DES (choline chloride/oxalic acid = 1:1) content was 168.1 g kg-1, extraction temperature was 79.8 °C, liquid-solid ratio was 23.3 mL g-1, and extraction time was 120 min, the maximum yield of 239.6 g kg-1 was obtained, which was almost twice the extraction of hot water. DES-extracted fig peel pectin (D-FP) exhibited better nature than hot water-extracted fig peel pectin (W-FP) in terms of uronic acid content, particle size distribution, and solubility, but lower molecular weight and esterification degree. D-FP and W-FP had similar infrared spectra and thermodynamic peaks but differed in monosaccharide compositions. D-FP also showed good antioxidant capacities and exhibited better functional activities than W-FP. These results indicated that D-FP was of promising quality being utilized in food or medical industries and the optimal DES-assisted extraction method might be applied as a sustainable process for the effective extraction of bioactive pectin from fig peels with the excellence of low equipment requirements and simple operation. © 2024 Society of Chemical Industry.

LC-HRMS-Driven Computational Toolbox to Assess Extraction Protocols Dedicated to Untargeted Analysis: How to Ease Analyzing Pesticide-Contaminated Soils?

Metabolomics is a powerful approach that allows for high throughput analysis and the acquisition of large biochemical data. Nonetheless, it still faces several challenging requirements, such as the development of optimal extraction and analytical methods able to respond to its high qualitative and quantitative requisites. Hence, the objective of the present article is to suggest a LC-HRMS-based untargeted profiling approach aiming to provide performant tools that help assess the performance and the quality of extraction methods. It is applied in a herbicide-contaminated soil metabolomics context. The trifactorial experimental design consists of 150 samples issued from five different extraction protocols, two types of soils, and three contamination conditions (contaminated soils with two different formulated herbicides against uncontaminated soils). Four performance and quality criteria are investigated using adapted LC-HRMS-driven computational tools. First, 861 metabolic features are annotated, and then the width of metabolome coverage and quantitative performance of the five different extraction protocols are assessed in all samples using various optimized configurations of heatmaps as well as van Krevelen diagrams. Then, the reproducibility of LC-HRMS profiles issued from the five extractions is studied by two different approaches: Euclidean distances and relative standard deviations. The two methods are examined and compared. Their advantages and limitations are thus discussed. After, the capacity of the different extractions to discriminate between contaminated and uncontaminated soils will be evaluated using orthogonal projections to latent structures-discriminant analysis. Different data scaling parameters are tested, and the results are explored and discussed. All of the suggested computational and visualization tools are performed using public-access platforms or open-source software. They can be readapted by metabolomics developers and users according to their study contexts and fields of application.

Response surface methodology optimization of extraction and enrichment conditions of total triterpenoid saponins from Celosiae Semen and evaluation of its lipid-lowering activity.

The saponin-enriched extract from Celosiae Semen is a promising resource owing to its lipid-lowering activity. However, triterpenoid saponins are difficult to extract owing to their high molecular weight and strong water solubility. The aim of this paper was to explore an eco-friendly and effective technology of extraction and enrichment of total triterpenoid saponins to obtain high lipid-lowering fractions. Initially, Box-Behnken design experiments were employed to optimize the heat reflux extraction process on the basic of mono-factor experiments. Afterwards, the crude extract was further purified using D-101 resin, and the purification parameters were investigated based on adsorption/desorption experiments and biological activity assay. Under optimal conditions, the purity of the finally obtained total triterpenoid saponins was increased by 7.28-fold. The lipid-lowering activities of the six main triterpenoid saponins were evaluated in HepG2 cells induced by palmitic acid. The results of Oil Red O staining showed that the compounds all exhibited potential lipid-lowering activity. The structure-activity relationship analysis suggested that the oligosaccharide chain at C-28 played an essential role in their lipid-lowering activity and the substituent group at C-23 site also showed important effects. The optimal extraction and purification methods may facilitate the utilization of Celosiae Semen for the industrial production as a functional food and drug.

Optimization of welan gum extraction and purification using lysozyme and alkaline protease.

Welan gum, a natural polysaccharide produced by Sphingomonas sp. ATCC 31555, has attracted considerable attention in the scientific community due to its desirable properties. However, challenges, such as high viscosity, residual bacterial cells, carotenoids, and protein complexation, hinder the widespread application of welan gum. In this study, we established a method for the extraction and purification of welan gum using a synergistic approach with lysozyme and alkaline protease. Lysozyme hydrolysis conditions were optimized by applying response surface methodology, and the best results for bacterial cell removal were achieved at 11 000 U/g, 44°C, and pH 9 after 3h of treatment. Subsequently, we evaluated protein hydrolysis through computer simulation and identified alkaline protease as the most suitable enzyme. Through experimental investigations, we found that the optimal conditions for alkaline protease hydrolysis were 7500 U/g, 50°C, pH 10, and 600rpm. These conditions resulted in a sugar recovery rate of 76.1%, carotenoid removal rate of 89.5%, bacterial removal rate of 95.2%, and protein removal rate of 87.3% after 3h of hydrolysis. The purified welan gum exhibited high transparency and purity. Structural characterization and antioxidant activity evaluation revealed that enzymatically purified welan gum has potential application prospects. Our study provides valuable insights into the optimal method for the enzymatic extraction and purification of welan gum. Such a method is conducive to the development of the multiple potential applications of welan gum. KEY POINTS: • A novel process for the synergistic purification of welan gum using lysozyme and alkaline protease was established. • In silico virtual digestion was employed to select the purification enzyme. • Welan gum with high transparency and purity was obtained.

Evaluation of Polyphenolic Profile and Antioxidant Activity of Sea Buckthorn (Elaeagnus rhamnoides (L.) A. Nelson) Leaf and Berry Extracts Obtained via Optimized Microwave-Assisted and Accelerated Solvent Extraction

The aim of this study was to optimize parameters of microwave-assisted extraction (MAE) and accelerated solvent extraction (ASE) in terms of extraction temperature and time, microwave power and cycle numbers on the phenolic content of sea buckthorn leaves and berries, using 70% ethanol (v/v) as an extraction solvent. The characterization of phenolic composition in leaf and berry extracts obtained at optimal MAE and ASE conditions was performed with UPLC/ESI-MS2, while antioxidant activity was determined using the ORAC method. The optimal extraction conditions for MAE were 60 °C, 500 W and 15 min for leaves and 60 °C, 300 W, and 10 min for berries. The optimal extraction conditions for ASE from both leaves and berries were 120 °C, 15 min, and 3 cycles. Total phenolic content (TPC) in MAE and ASE extracts from leaves was similar to the TPC determined in extracts obtained by conventional extraction (60 °C/30 min); however, ASE contributed to the higher TPC of the berry extracts. The flavonols kaempferol-3-rutinoside in the leaves and kaempferol in the berries were the most abundant phenols of sea buckthorn. A higher antioxidant activity was found in the leaf extracts obtained by ASE and it correlated with the phenolic content. In general, ASE favored the extraction of all polyphenols from leaves, while MAE was more suitable for the extraction of flavonols from berries, suggesting that the choice of the optimal extraction method is crucial with regard to the target molecules and future applications.

Microwave-assisted extraction of Lawsonia inermis L. leaves: Method validation, optimization, and tyrosinase-stimulating activity

Vitiligo is a long-term skin condition characterized by the development of pale white patches due to a lack of melanin. Lawsonia inermis L. leaves, which contain lawsone, have been explored as a potential alternative treatment for vitiligo. This study aimed to optimize the microwave-assisted extraction of L. inermis leaves and evaluate its ability to stimulate tyrosinase activity, which is relevant to vitiligo treatment. The Box-Behnken design was employed, with three factors being varied: microwave power, time, and cycle. Two responses were monitored: extraction yield and lawsone content. To determine the lawsone content, validated high-performance liquid chromatography was utilized, which demonstrated good linearity, specificity, precision, and accuracy. The optimal conditions that provided the highest extraction yield and lawsone content were then used to evaluate the extract’s ability to stimulate tyrosinase activity. The results revealed that a microwave power of 300 W and a microwave time of 20 s for one cycle yielded an extraction yield of 12.99% ± 0.10% and a lawsone content of 94.85 ± 3.12 mg/g extract. The accuracy of the prediction, with a percent error of less than 10%, confirmed the reliability of the computer program used for data prediction. Furthermore, the extract exhibited significant stimulation of tyrosinase activity, indicating its potential usefulness in vitiligo treatment. The optimal microwave-assisted extraction method identified in this study holds promise for maximizing extraction yield and lawsone content in L. inermis leaves extract. This extract could serve as a basis for developing topical products for the treatment of vitiligo.

Preparation of imidazole-modified paper membrane for selective extraction of gallic acid and its structural and functional analogues from Pomegranate Peel.

In the search for pharmaceutically active compounds from natural products, it is crucial and challenging to develop separation methods that target not only structurally similar compounds but also a class of compounds with desired pharmaceutical functions. To achieve both structure-oriented and function-oriented selectivity, the choice of functional monomers with broad interactions or even biomimetic roles towards targeted compounds is essential. In this work, an imidazole (IM)-functionalized paper membrane was synthesized to realize selectivity. The IM was selected based on its capability to provide multiple interactions, participation in several bioprocesses, and experimental verification of adsorption performance. Using gallic acid as a representative component of Pomegranate Peel, the preparation conditions and extraction parameters were systematically investigated. The optimal membrane solid-phase extraction (MSPE) method allowed for enrichment of gallic acid from the complex matrix of Pomegranate Peel, enabling facile quantitative analysis with a limit of detection (LOD) of 0.1 ng mL-1. Furthermore, with the aid of cheminformatics, the extracted compounds were found to be similar in both their structures and pharmaceutical functions. This work offers a novel approach to preparing a readily synthesized extraction membrane capable of isolating compounds with similar structures and pharmaceutical effects, and provides an MSPE-based analytical method for natural products.

Classifying Routine Clinical Electroencephalograms With Multivariate Iterative Filtering and Convolutional Neural Networks.

Electroencephalogram (EEG) is widely used in basic and clinical neuroscience to explore neural states in various populations, and classifying these EEG recordings is a fundamental challenge. While machine learning shows promising results in classifying long multivariate time series, optimal prediction models and feature extraction methods for EEG classification remain elusive. Our study addressed the problem of EEG classification under the framework of brain age prediction, applying a deep learning model on EEG time series. We hypothesized that decomposing EEG signals into oscillatory modes would yield more accurate age predictions than using raw or canonically frequency-filtered EEG. Specifically, we employed multivariate intrinsic mode functions (MIMFs), an empirical mode decomposition (EMD) variant based on multivariate iterative filtering (MIF), with a convolutional neural network (CNN) model. Testing a large dataset of routine clinical EEG scans (n = 6540) from patients aged 1 to 103 years, we found that an ad-hoc CNN model without fine-tuning could reasonably predict brain age from EEGs. Crucially, MIMF decomposition significantly improved performance compared to canonical brain rhythms (from delta to lower gamma oscillations). Our approach achieved a mean absolute error (MAE) of 13.76 ± 0.33 and a correlation coefficient of 0.64 ± 0.01 in brain age prediction over the entire lifespan. Our findings indicate that CNN models applied to EEGs, preserving their original temporal structure, remains a promising framework for EEG classification, wherein the adaptive signal decompositions such as the MIF can enhance CNN models' performance in this task.

Indium Recovery from End-of-Life E-Waste: Important Details Related to Spectroanalytical Determination and Recycling Viability

Recycling has experienced great interest over the past five years, primarily driven by its strategic economic significance and the growing scarcity of natural resources. One element that has garnered attention is indium (In), especially due to its presence in flat panel displays (FPDs), particularly in devices utilizing liquid crystal display (LCD). The goal of this research was to establish a method for extracting In from LCD. The study faced challenges related to In determination using inductively coupled plasma optical emission spectroscopy (ICP OES), and furthermore, it proposed an optimized extraction method through design of experiments (DoE), focusing on extraction time and percentage of solid variables. Diverse sample types encompassing smartphones, monitors, and television screens were processed. Leaching was conducted utilizing a magnetic plate at 80 °C, employing a 1 mol L-1 H2SO4 solution along with 25% m v-1 of the sample. This proposed method achieved a near-complete extraction rate (100%) for In. Moreover, in-depth interviews were conducted with several stakeholders in urban mining and various sectors within Brazil. The insights gleaned from these interviews showed the absence of a consolidated market for recycling LCDs with a specific emphasis on In recovery.

Screening and identifying natural products with SARS-CoV-2 infection inhibitory activity from medicinal fungi

The coronavirus disease of 2019 (COVID-19), a global pandemic caused by the severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2), can result in severe health complications. In addition to physical preventative measures, pharmaceutical intervention is also crucial. Numerous natural products from medicinal fungi have shown promise as potential antiviral drugs and may serve as a source of effective components with antiviral activity against SARS-CoV-2 and other coronaviruses. In this study, we developed a workflow that integrates viral infection inhibition assays at both cellular and molecular levels, as well as molecular separation and characterization, to screen and identify natural products with antiviral activity. Using this workflow, we screened 167 extracts extracted from 36 medicinal fungi using optimized extraction methods. We assessed the antiviral effects of these extracts by measuring their ability to inhibit SARS-CoV-2 infection and receptor binding domain - human angiotensin-converting enzyme 2 (RBD-hACE2) binding in vitro. Following charge- and size-based characterization of the active compounds through filtration and chromatographic fractionation, mass spectrometry characterization of the fractionated compounds revealed that the active components are polysaccharides and determined their monosaccharide residue composition. Our findings provide new insights into the antiviral potential of natural products and their screening strategies and may contribute to the development of effective antiviral therapeutics against COVID-19 and other diseases.

Exploring the potential of Salicornia: A halophyte’s impact on Agriculture, the Environment, and the Economy

Salicornia, a halophytic plant, garners attention for its environmental, energy, medicinal, and economic potential. It excels in environmental management through phytoremediation and carbon sequestration, thriving in saline environments to filter toxins and recycle nutrients. As a biofuel source, its oil-rich seeds and high biomass yield offer eco-friendly alternatives for biodiesel and bioethanol production, mitigating greenhouse gas emissions. Salicornia’s bioactive compounds exhibit significant potential in modulating the immune system and managing various diseases. Despite challenges such as production costs and regulatory barriers, Salicornia holds promise as a sustainable crop with diverse commercial applications. Scaling up Salicornia production and utilization requires addressing challenges related to cultivar development, production costs, and regulatory frameworks. However, with continued research and investment, Salicornia could emerge as a valuable resource for addressing food security, energy sustainability, and environmental restoration. Future research directions include exploring Salicornia’s nutritional composition, environmental sustainability, and epigenetic mechanisms, as well as optimizing extraction methods and intercropping systems. Understanding these aspects will contribute to unlocking Salicornia’s full potential as a versatile crop with wide-ranging benefits for human health, environmental conservation, and economic development.

Effects of different drying, extraction methods, and solvent polarity on the antioxidant properties of Paeonia daurica subsp. mlokosewitschii leaves

The study presents the effect of drying methods (microwave-drying and freeze-drying), different solvents (80% methanol, 99% methanol, 80% ethanol), and different extraction methods on the antioxidant activity of Paeonia daurica subsp. mlokosewitschii leaves, estimated based on DPPH free radical scavenging activity. The highest antioxidant activity was revealed in the freeze-dried leaves. The drying method significantly influenced the antioxidant activity: the thermal microwave-drying resulted in lower antioxidant potential. The solvent polarity also played a significant role in the determination of the antioxidant activity of Paeonia daurica subsp. mlokosewitschii leaves: the lowest IC50 values (specific concentration of the sample required for 50% inhibition) were revealed for freeze-dried plants extracted with 80% methanol, followed by IC50 values obtained for the extraction with 80% ethanol, and the highest IC50 values were revealed for extracts of microwave-dried plants extracted with 99% methanol. The subsequent drying of freeze-dried plant extracts had no significant effect on the antioxidant activity of the extract. The subsequent drying of the methanol extract from microwave-dried plants at room temperature or 40°C significantly reduced IC50 value, however, the results were comparable with those, obtained for the methanol extracts of freeze-dried plants without subsequent drying of the extract. Thus, the optimal method of drying and extraction of Paeonia daurica subsp. mlokosewitschii leaves for preserving the antioxidant activities was established: freeze-drying of leaves followed by 24 h extraction with 80% methanol.

The Effect of Dietary Supplementation with Haematococcus pluvialis for Enhanced Pigmentation in Amphiprion ocellaris

Among the minority seawater species in the ornamental fish market, clownfish (Amphiprion ocellaris) have a high market value due to their vibrant appearance. Astaxanthin, a promising coloring agent, is applied in diets as a food additive to enhance the physical appearance of clownfish. However, as the retail price of astaxanthin has been inflating, the industry is eager to find more affordable astaxanthin products. The present study evaluated the nutrients and pigmentation performance of the algae-extracted astaxanthin diets of clownfish, followed by a comparative feeding trial evaluating the graded levels of either Haematococcus pluvialis powder or extracted astaxanthin supplements in the experimental diets. The study included three stages: assessing the utilization of H. pluvialis powder as an astaxanthin source, investigating the optimal practical extraction method, and revisiting the effects of crude extracted astaxanthin on clownfish based on the identified preparation processes. In the first stage, H. pluvialis powder was applied as the feed additive for a feeding trial, resulting in a low-utilization rate of astaxanthin in clownfish. This indicated that a suitable extraction method was essential for clownfish. Two chemical-based methods for astaxanthin extraction were investigated to obtain the optimal extraction yields; results showed that the HCl–acetone method had an astaxanthin yield of 21.99 ± 0.52 mg/g cell, which was significantly higher than the yield from the acetic acid-DMSO method. Finally, the effects of HCl–acetone-extracted astaxanthin was compared with the effects of synthesized astaxanthin. The pigmentation performance study was performed using a digital image acquisition and processing technique. A significant increase in the red color signal was observed at week six after fed with 400 and 200 mg/kg of the extracted astaxanthin, compared to the control 0 mg/kg. In conclusion, H. pluvialis-extracted astaxanthin following the HCl–acetone method can significantly improve the pigmentation performance of A. ocellaris after 42 days of oral administration.

Optimization of the Extraction of Bioactive Compounds from Cabernet Sauvignon Grape Pomace from Querétaro, Mexico, Using MSPD

Red wine contains polyphenols which are extracted during the winemaking process. However, winemaking is not an extraction; therefore, the resulting byproducts still have a substantial polyphenol content. The aim of this study was to compare two methods for the extraction of phenolic compounds: maceration and matrix solid-phase dispersion (MSPD). Grape pomace (Vitis vinifera var. Cabernet Sauvignon) from a winery in Querétaro, Mexico was used. The optimal conditions for both methods were identified. Phenolic compounds and antioxidant activity were the response variables. A central composite design was used (Minitab 17) for the extraction by maceration. The maceration time (1, 4, 12, 20, and 24 h) and the ratio of ethanol (50 to 80%) acidified with 1% HCl were the two factors studied. For the MSPD extraction, sea sand was used as a dispersant, and a 22 factorial design was employed for the evaluation, with the elution volume and the ratio of sample/dispersant being the two factors analyzed. The optimal extraction method was MSPD with 96 mL (acidified ethanol) as the elution volume and a 1:2 ratio of sample/dispersant. Using these conditions, 14.01 ± 0.19 mMol TEAC/100 g db (Trolox equivalent of antioxidant capacity) of grape pomace was obtained, whereas the total phenolic content was 2836.73 ± 41.90 mg GAE/100 g db. These values are greater than those obtained by maceration. These conditions are close to those predicted by the model (analysis of variance (ANOVA) with a level of significance of 5% (p < 0.05) and a Tukey comparison test for determining significant differences in the comparison of results).

Method Development for Aminopyralid Residues Determination by Ultra-High-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry in Straw

Straw is an important by-product of crop production. It has been widely used as a feed as well as in fruit–vegetable production due to exerting a positive impact on soil and crop health and quality in the operated areas. On the other hand, applied crop-specific herbicides throughout the production stage, like aminopyralid (AP), may lead to significant plant injuries in sensitive vegetable plantations, even in very low concentrations. This study aims to optimize a short time, minimal consumables needed, and sensitive extraction and analytical method for AP residues in straw material using LC-MS/MS. For this purpose, standard AP signal response in acetonitrile (MeCN) and 1% of formic acid (FA) in methanol (MeOH) were tested; several chromatographic separation and mass spectroscopy (MS) parameters were improved and optimized. Subsequently, two different extraction methods were performed in AP spiked straw samples, and extraction efficacies were compared. Salting-out assisted liquid–liquid extraction (SALLE) by acidified MeCN combined with final dissolution in MeOH with 1% of FA prior to the analysis was chosen as the most appropriate method for the straw matrix. This method was then used for validation and real sample test analysis. The limit of quantification (LOQ) of AP in this optimized extraction method achieved 10 ng/g straw with a recovery rate of 71% and 13% RSD. The method was also tested on field straw mulch samples and 22.54 ± 0.8 ng/g of AP was detected.

Extraction, Phytochemical Screening and HPTLC Analysis of Fenugreek Gum for Analysis of Different Phytoconstituents

Fenugreek gum is a natural polysaccharide that has been explored for various biomedical applications. The present study investigated the phytoconstituent profile of fenugreek gum, revealing it as a potent source of diverse bioactive compounds. The analysis encompassed steroids, fats and oils, alkaloids, proteins, saponins, tannins, phenolics, flavonoids, and carbohydrates. Extraction using methanol and aqueous solvents demonstrated the highest concentration of phytoconstituents, underscoring the efficacy of these solvents in isolating bioactive components from fenugreek. Further exploration involved the determination of Rf values and percentage area in chloroform, petroleum ether, and chloroform extracts, providing a comprehensive identification of the mixture’s components. The results suggested a rich and varied chemical composition in fenugreek gum, offering potential applications in diverse fields owing to the presence of steroids for physiological effects, fats and oils for nutritional benefits, alkaloids with potential pharmacological properties, proteins for cellular functions, saponins for their soap-like properties, and tannins and phenolics as antioxidants. Additionally, the presence of flavonoids and carbohydrates adds to its nutritional and medicinal value. The study’s findings contribute valuable insights into the phytochemical composition of fenugreek gum, shedding light on its potential applications in the realms of medicine, nutrition, and industry. The identification of optimal extraction methods and the characterization of phytoconstituents lay the foundation for future research and utilization of fenugreek gum as a versatile and valuable natural resource. Overall, this investigation underscores the significance of fenugreek gum as a rich repository of bioactive compounds with diverse potential applications across various domains.