Min Extraction Time Research Articles

Comprehensive Analysis and Environmental Risk Assessment of Benzotriazoles in Airport Stormwater: A HS-SPME-GC × GC-TOF-MS-Based Procedure as a Tool for Sustainable Airport Runoff Water Management

Despite the numerous benefits of intensive air transport development, many activities associated with the operation of airports contribute to environmental pollution. The purpose of this research was the development, optimization, and validation of a headspace–solid-phase microextraction–comprehensive two-dimensional gas chromatography–time of flight–mass spectrometry (HS-SPME-GC × GC-TOF-MS)-based procedure for determining anti-corrosive compounds in airport stormwater. Optimized HS-SPME conditions include: 45 min extraction time, 100 °C temperature, 1.0 g salt addition, and 10 min desorption time at 270 °C. The developed procedure is sensitive, selective, accurate (recoveries ≥ 80.0%), and precise (the coefficient of variation (CV) ≤ 14.9%), making it a highly suitable tool for extensive airport stormwater quality monitoring. The validated analytical protocol was successfully used to detect pollutants, including 1H-BT, 4-MeBT, 5-MeBT, and 5,6-diMe-1H-BT, in stormwater from various European airports with different flight capacities. Throughout the sampling period at the investigated airports, 1H-benzotriazole was found in the highest concentrations, ranging from below the MQL to 467 mg/L. An ecotoxicological risk assessment revealed that 69% of the sites exhibited high risk levels (Risk Quotient ≥ 1). The developed procedure and carried out environmental risk assessments of benzotriazoles in airport stormwater enable an evidence-based approach to sustainable airport stormwater management.

Determination of six short‐chain fatty acids in rat feces using headspace solid‐phase dynamic extraction coupled with GC‐MS

Short‐chain fatty acids (SCFAs) are organic acids with carbon atoms less than six, released through fermentation products by intestinal microbiome, having multiple physiological activities. Considering weak acidity and high volatility, derivatization or liquid–liquid extraction is essential, which is time consuming. Headspace‐solid‐phase dynamic extraction (HS‐SPDE) coupled with gas chromatography‐mass spectrometry is automated and effortless to determine SCFAs in rat feces. The extraction procedure is performed by aspirating and discharging the headspace cyclically through a steel needle, coated with an inner polyethylene glycol sorbent. The key parameters of SPDE were optimized including coating type, incubation time and temperature, and number of extraction strokes. Besides, salting‐out was conducted. Then, a method by HS‐SPDE‐GC‐MS was established and validated. It only took 3‐min incubation time, 4.5 min extraction time, and 13 min chromatographic separation in a run. The recovery, linearity, limit of quantification, and stability were evaluated. Then, the proposed method was applied to analyze rat feces including 18 rats with liver injury and 23 normal controls. Mann–Whitney U test indicated that the concentrations of six SCFAs in normal rat feces were higher than those with liver injury. This method provides a choice for fast, solvent‐free, automated, and high‐throughput analysis of SCFAs.

Enhancing the Nutritional Profile of Crataegus monogyna Fruits by Optimizing the Extraction Conditions

Crataegus monogyna (CM) fruits are highly regarded for their rich nutritional content, boasting elevated levels of various beneficial secondary metabolites like total polyphenols, including anthocyanins, and ample amounts of ascorbic acid and antioxidant activity. Despite the acknowledged benefits of CM fruits, researchers have directed more attention toward its leaves and flowers. Consequently, the current research attempts to optimize extraction techniques for CM fruit using a multifaceted approach involving varied durations, temperatures, and concentrations of ethanol solvent to isolate the diverse range of bioactive components present effectively. High-performance liquid chromatography coupled with a diode array detector (HPLC-DAD) is employed for the identification and quantification of polyphenolic compounds. According to the results, by following the optimum extraction parameters (50% ethanolic solvent, 50 °C extraction temperature, and 60 min extraction time), the total polyphenol content can be increased up to 410%, reaching 55.59 mg gallic acid equivalents/g. Using 50% ethanolic solvent, 80 °C extraction temperature, and extraction time of 90 min, the total anthocyanin content can be enhanced by more than 560%, reaching a quantity of 51.83 μg cyanidin equivalents/g. Moreover, the antioxidant activity of CM fruit extracts can reach 415.95 μmol ascorbic acid equivalents (AAE)/g dw (by FRAP method), using 50% ethanolic solvent, 50 °C extraction temperature, and 60 min extraction time, and 270.26 μmol AAE/g dw (by DPPH method) and 1053.28 mg/100 g dw ascorbic acid content, using 50% ethanolic solvent, 80 °C extraction temperature, and 90 min extraction time. This comprehensive study seeks to augment the already substantial content of bioactive compounds found in CM, resulting in an extract with promising applications across the pharmaceutical, food, and cosmetics industries.

Optimization of the Parameters Influencing the Antioxidant Activity and Concentration of Carotenoids Extracted from Pumpkin Peel Using a Central Composite Design.

It has been discovered that the peel of a pumpkin (Cucurbita maxima), regarded as a waste product of pumpkin processing, has significant amounts of carotenoids and other antioxidants. This study aims to identify the most effective extraction parameters for an ultrasonic-assisted extraction method to extract the total carotenoids (TCs) and assess the antioxidant activity (AA) of pumpkin peel. To determine the effects of the extraction time, temperature, and material-to-solvent ratio on the recovery of TCs and AA, a response surface methodology utilizing the central composite design (CCD) was used. The extraction temperature (6.25-98.75 °C), extraction duration (13.98-128.98 min), and solvent ratio (0.23-50.23 mL) were the variables studied in the coded form of the experimental plan. The carotenoid concentration varied from 0.53 to 1.06 mg/g DW, while the AA varied from 0.34 to 7.28 µM TE/g DW. The findings indicated that the optimal extraction parameters were an 80 °C temperature, a 10 mL solvent ratio, and a 100 min extraction time. The study confirmed that the optimum extraction conditions resulted in an experimental TC yield of 0.97 mg/g DW and an AA of 7.25 µM TE/g DW. Overall, it should be emphasized that the extraction process can be enhanced by setting the operating factors to maximize the model responses.

Solvent Bar Microextraction Method Based on a Natural Deep Eutectic Solvent and Multivariate Optimization for Determination of Steroid Hormones in Urine and Water

Steroid hormones may pose potential risks to both human health and wildlife, primarily through the consumption of medication or polluted food and water; efforts are being made to monitor their levels in the human body and regulate and minimize their releases to the environment. In this study, a simple and environmentally friendly sample preparation method was developed to simultaneously determine three steroid hormones in urine and water samples. A monoterpene (menthol) and a fatty acid (lauric acid) were combined in various ratios to form a hydrophobic deep eutectic (HDE) solvent as an extraction solvent in solvent bar microextraction (SBME). Using a univariate strategy, a menthol-to-lauric acid HDE ratio of 4:1 and a pH 7 of the sample solution resulted in the highest extraction efficiency (EE%) of the selected steroids. The computational methods have been employed to predict a 4:1 HDE interaction with chosen steroids. Additionally, chemometric approaches suggested that the optimal extraction conditions involved HDEs as extract solvent confined within three SBME devices directly immersed into a 20 mL sample solution with a 30 min extraction time, followed by ultrasonication within 200 μL of elution solvent for a 5 min elution time. Under optimized conditions, the method calibration graph for the spiked selected steroids in the water and urine samples showed good linearity with R2 ≥ 0.994 with limits of detection/quantification lower than 0.40/1.35 μg L−1 and repeatability/reproducibility (RSD%, n = 5) lower than 5.09/7.11. The developed method allows a safe, rapid, and reliable analysis of three steroid hormones in human urine and water samples without using toxic volatile organic solvents.

Quantitative analysis of organosulphur compounds in crude oil samples using magnetic solid phase extraction based on Au-Fe3O4 adsorbent and gas chromatography with time-of-flight mass spectrometry

This study focused on the development of a magnetic solid phase extraction (m-SPE) method using Au-Fe3O4 as an adsorbent followed by GC-ToFMS analysis for the determination of organosulphur compounds (OSCs) in fuel samples. The m-SPE using Au-Fe3O4 NPs was preferred because of the low toxicity of the adsorbent1, high separation efficiency using external magnet2 and greater extraction selectivity between sulphur and Au atom3. The Au-Fe3O4 NPs were characterized using XRD, UV–Vis, TEM, SEM and FTIR. This method was optimized using multivariate analysis based on a two-level full factorial and central composite designs. The conditions which produced optimum efficiency were found to be 150 mg mass of sorbent, 100 µL eluent volume, 50 min extraction time and 6,5 pH of the sample. These optimum conditions showed a relatively low limit of detection in the range of 0.02–0.199nµg/g and limit of quantification of 0.08–0.602 µg/g. Furthermore, a relative standard deviation of triplicates analysis was between 0.8 and 2.3% with good linearity of 0.9816–0.9961. The percentage recovery for thiophene, 3-methylthiophene, benzothiophene and dibenzothiophene ranged from 76 to 95% for the spiked samples. The optimized m-SPE method was then applied in real fuel oil samples. The concentration of thiophene, 3-methylthiophene, benzothiophene and dibenzothiophene in crude oil, gasoline, diesel and kerosene ranged from 0.43–1.94 µg/g, 0.78–1.63 µg/g, 0.95–4.31 µg/g to 1.55–2.09 µg/g, respectively. The m-SPE, followed by GC-ToFMS method, proved to be efficient, inexpensive and an alternative method for OSCs analysis in fuel oils.

Safflower protein as a potential plant protein powder: optimization of extraction and spray-drying process parameters and determination of physicochemical and functional properties.

The research about sustainable and alternative plant protein sources has accelerated with the increasing need for protein. Safflower meal has a potential to be used in protein production due to its high protein content. This research aimed to produce an alternative plant-based protein powder using safflower meal. Both extraction and spray-drying parameters of safflower protein powder production were optimized using response surface methodology to achieve maximum yield. Moreover, the physicochemical and functional properties of safflower protein were determined and compared with those of commercial protein powders (soy, sunflower, pea, fava bean, and rice). The optimum extraction conditions were found to be 33.06:1 mL-1 g solvent-to-meal ratio, pH 11.00, 23.34 °C extraction temperature, and 30.86 min extraction time, which were achieved with a protein yield response of 75.21%. The highest powder yield (51.28%) was recorded for drying conditions of inlet air temperature of 160.11 °C, aspiration rate of 54.17 m3 h-1, and feed flow rate of 16.01 mL min-1. According to the amino acid profile of safflower protein, the glutamic acid content (14 475 mg (100 g)-1) was highest, while the methionine content (96 mg (100 g)-1) was lowest. Moreover, safflower protein can be regarded as a high-quality protein due to its high essential amino acid ratio (41.55%). The experiments showed that safflower protein had high solubility and good foam and emulsifying properties. Safflower protein could be a nutritional and functional protein source for the food industry. © 2024 Society of Chemical Industry.

Box-Behnken Design-Based Optimization of Phytochemical Extraction from Diplazium esculentum (Retz.) Sw. Associated with Its Antioxidant and Anti-Alzheimer's Properties.

A previous study reported that the ethanolic extract of the edible fern, Diplazium esculentum (Retz.) Sw. (DE), obtained from a non-optimized extraction condition exhibited anti-Alzheimer's disease (AD) properties through the inhibition of a rate-limiting enzyme in amyloid peptide formation, β-secretase-1 (BACE-1). Nevertheless, a non-optimized or suboptimal extraction may lead to several issues, such as a reduction in extraction efficiency and increased time and plant materials. In this study, extraction of the DE was optimized to obtain appropriate BACE-1 inhibition using a Box-Behnken design (BBD) and response surface methodology (RSM). Data revealed that the optimal extraction condition was 70% (v/v) aqueous ethanol, 50 min extraction time, 30 °C extraction temperature, and 1:30 g/mL solid/liquid ratio, giving BACE-1 inhibition at 56.33%. In addition, the extract also exhibited significant antioxidant activities compared to the non-optimized extraction. Metabolomic phytochemical profiles and targeted phytochemical analyses showed that kaempferol, quercetin, and their derivatives as well as rosmarinic acid were abundant in the extract. The optimized DE extract also acted synergistically with donepezil, an AD drug suppressing BACE-1 activities. Data received from Drosophila-expressing human amyloid precursor proteins (APPs) and BACE-1, representing the amyloid hypothesis, showed that the optimized DE extract penetrated the fly brains, suppressed BACE-1 activities, and improved locomotor functions. The extract quenched the expression of glutathione S transferase D1 (GSTD1), inositol-requiring enzyme (IRE-1), and molecular chaperone-binding immunoglobulin (Bip), while donepezil suppressed these genes and other genes involved in antioxidant and endoplasmic reticulum (ER) stress response, including superoxide dismutase type 1 (SOD1), activating transcription factor 6 (ATF-6), and protein kinase R-like endoplasmic reticulum kinase (PERK). To sum up, the optimized extraction condition reduced extraction time while resulting in higher phytochemicals, antioxidants, and BACE-1 inhibitors.

Ultrasonic-Assisted Extraction of Xanthorrhizol from Curcuma xanthorrhiza Roxb. Rhizomes by Natural Deep Eutectic Solvents: Optimization, Antioxidant Activity, and Toxicity Profiles.

Xanthorrhizol, an important marker of Curcuma xanthorrhiza, has been recognized for its different pharmacological activities. A green strategy for selective xanthorrhizol extraction is required. Herein, natural deep eutectic solvents (NADESs) based on glucose and organic acids (lactic acid, malic acid, and citric acid) were screened for the extraction of xanthorrhizol from Curcuma xanthorrhiza. Ultrasound-assisted extraction using glucose/lactic acid (1:3) (GluLA) gave the best yield of xanthorrhizol. The response surface methodology with a Box-Behnken Design was used to optimize the interacting variables of water content, solid-to-liquid (S/L) ratio, and extraction to optimize the extraction. The optimum conditions of 30% water content in GluLA, 1/15 g/mL (S/L), and a 20 min extraction time yielded selective xanthorrhizol extraction (17.62 mg/g) over curcuminoids (6.64 mg/g). This study indicates the protective effect of GluLA and GluLA extracts against oxidation-induced DNA damage, which was comparable with those obtained for ethanol extract. In addition, the stability of the xanthorrhizol extract over 90 days was revealed when stored at -20 and 4 °C. The FTIR and NMR spectra confirmed the hydrogen bond formation in GluLA. Our study reported, for the first time, the feasibility of using glucose/lactic acid (1:3, 30% water v/v) for the sustainable extraction of xanthorrhizol.

Optimization of Combined Microwave and Ultrasound Extractions of Cannabinoids Compounds from Cannabis indica L. (Blueberry Cultivar) Using Response Surface Methodology

Microwave and ultrasound are novel technologies that are widely used for extracting bioactive compounds from plant materials. In this study, combined extraction techniques, microwave and ultrasound, were applied to extract cannabinoids, cannabidiol (CBD) and delta-9-tetrahydrocannabinol (THC), from Cannabis indica L. (Blueberry cultivar). Three independent variables including solid to liquid ratio (X1, A: 1:10-1:30 w/v), microwave extraction time (X2, B: 5-20 min), and ultrasound extraction time (X3, C: 10-30 min) were optimized using central composite design (CCD). The experimental data obtained was fitted to a second-order polynomial equation using multiple regression analysis and additionally analyzed using appropriate statistical methods (analysis of variance, ANOVA). The optimum conditions were determined according to the solid to liquid ratio (X1, A) of 1:22 (w/v), microwave extraction time (X2, B) of 5 min and ultrasound extraction time (X3, C) of 14 min. Under these conditions, the experimental CBD and THC content was 0.298±0.001 mg/g dry weight and 91.35±0.35 mg/g dry weight, respectively. The experimentally-achieved values were in accordance with those estimated by the CCD model, suggesting the applicability of the utilized model and the favorable result of CCD’s application in the optimization of the combined microwave and ultrasound extraction.

Urinary biomonitoring of fuel ether oxygenates using a needle trap device packed with a novel molecularly imprinted polymer surface modified Zeolite Y

This study introduces an innovative needle trap device (NTD) featuring a molecularly imprinted polymer (MIP) surface-modified Zeolite Y. The developed NTD was integrated with gas chromatography-flame ionization detector (GC-FID) and employed for analysis of fuel ether oxygenates (methyl tert‑butyl ether, MTBE, ethyl tert‑butyl ether, ETBE, and tert‑butyl formate, TBF) in urine samples. To optimize the key experimental variables including extraction temperature, extraction time, salt concentration, and stirring speed, a central composite design-response surface methodology (CCD-RSM) was employed. The optimal values for extraction in the study were found to be 51.2 °C extraction temperature, 46.2 min extraction time, 27 % salt concentration, and 620 rpm stirring speed. Under the optimized conditions, the calibration curves demonstrated excellent linearity within the range of 0.1–100 μg L−1, with correlation coefficients (R2) exceeding 0.99. The limits of detection (LODs) for MTBE, ETBE, and TBF were obtained 0.06, 0.08, and 0.09 μg L−1, respectively. Moreover, the limits of quantification (LOQs) for MTBE, ETBE, and TBF were obtained 0.18, 0.24, and 0.27 μg L−1, respectively. The enrichment factor was also found to be in the range of 98–129.The NTD-GC-FID procedure demonstrated a high extraction efficiency, making it a promising tool for urinary biomonitoring of fuel ether oxygenates with improved sensitivity and selectivity compared to current methods.

Optimization of Red Ginger (Zingiber officinale var. Rubrum) Extraction Using Microwave Assisted Hydrodistillation Method

Red ginger is a spice plant that has high economic and social value. One of the uses of red ginger is to process it into a product, namely essential oil. This study aims to determine the optimization of the extraction process conditions on solvent volume, time, and extraction power that can produce optimum yield and residual content of red ginger essential oil solvent. The extraction was carried out with the help of microwaves. The research method is experimental design and optimization process with Response Surface Methodology (RSM) type Box-Behnken Design (BBD). The results showed that the optimum yield was at 700 mL solvent volume, 1 min extraction time, and 10% power (69.9 watts) with the equation Y = 0.2076 + 0.0262A – 0.0300B – 0.0013C and the concentration conditions the optimum remaining solvent with the equation Y = 4.98 – 1.0000A + 4.56B + 5.44C. The optimal yield of red ginger essential oil was 0.205%, with a residual solvent content of 3.8%, specific gravity 0.885, acid number 1.399, refractive index 1.485. The results of the optimum residual solvent content of -6.023%. Based on the results obtained, the yield value with the help of microwaves is higher than that without the help of microwaves. Keywords: Essential oil, Microwave, Residual solvent content, Response surface methodology (RSM), Yield.

Analysis of Three Dimethyl Sulfides in Freshwater Lakes Using Headspace Solid-Phase Microextraction-Gas Chromatography with Flame Photometric Detection

Dimethyl sulfides are ubiquitous odorous substances in eutrophic freshwater bodies. In this study, a simple headspace solid-phase microextraction-gas chromatography-flame photometric detection method was developed to detect three representative algal-derived dimethyl sulfides in freshwater lake water samples: dimethyl monosulfide (DMS), dimethyl disulfide (DMDS), and dimethyl trisulfide (DMTS). The effects of extraction fiber, temperature, pH, ionic strength, and sample volume were investigated orthogonally, and the optimized method was applied to analyze surface water samples from Lake Ulansuhai in Inner Mongolia, China. Optimal extraction was obtained with a 50/30 µm DVB/CAR/PDMS extraction fiber, 20% ion concentration, 87 min extraction time, and 50 °C extraction temperature. The correlation coefficients of the standardized working curves for DMS, DMDS, and DMTS were 0.9967, 0.9907, and 0.9994, respectively, indicating good linear relationships. Limits of detection were in the nanogram range, and the recoveries of the spiked standards for DMS, DMDS, and DMTS were 97.22~99.07%, 93.39~99.34%, and 91.17~99.25%, with relative standard deviations of 5.18~5.94%, 3.08~6.25%, and 2.56~5.47%, respectively. This method is stable and reliable, and can be used for the determination of volatile sulfides in freshwater lake water.

Optimizing ultrasonic-assisted extraction and untargeted metabolite identification from red water lily (Nymphaea rubra) leaves with enhanced antioxidant activity

This study aimed to optimize the ultrasonic-assisted extraction of polyphenolic compounds from red water lily (Nymphaea rubra) leaves (NRL) with heightened antioxidant activities and perform untargeted metabolite identification. Response surface methodology, employing Box-Behnken design, determined optimal conditions: 53.0 % ethanol, 32.0 min extraction time, and 53.0 °C temperature. The resulting extraction demonstrated significant total phenolic content of 45.12 ± 1.12 mgGAE/g and total flavonoid content of 44.05 ± 1.65 mgCAE/g. High-resolution mass spectrometry identified 150 secondary metabolites, encompassing phenols, flavonoids, tannins, terpenoids, and fatty acids. The optimized NRL extract exhibited notably increased radical scavenging abilities (19.21 ± 1.71 μM ASCE/g for DPPH and 24.59 ± 1.35 μM ASCE/g for ABTS) along with elevated reducing power potential (63.35 ± 4.28 μM ASCE/g for CUPRAC and 61.32 ± 2.56 μM ASCE/g for FRAP) in comparison to traditional extracts, which ranged from (7.23 ± 1.58 to 15.13 ± 1.79 μM ASCE/g, 13.29 ± 1.32 to 19.29 ± 1.69 μM ASCE/g, 22.74 ± 1.68 to 54.37 ± 3.38 μM ASCE/g, 24.14 ± 2.00 to 52.77 ± 2.33 μM ASCE/g for DPPH, ABTS, CUPRAC and FRAP, respectively). This suggests its promising potential for incorporation into antioxidant-rich functional foods. These findings underscore NRL's promise for commercial applications in the nutraceutical, food, and pharmaceutical industries.

Deep eutectic solvent-based shaking-assisted extraction for determination of bioactive compounds from Norway spruce roots.

Polyphenolic compounds play an essential role in plant growth, reproduction, and defense mechanisms against pathogens and environmental stresses. Extracting these compounds is the initial step in assessing phytochemical changes, where the choice of extraction method significantly influences the extracted analytes. However, due to environmental factors, analyzing numerous samples is necessary for statistically significant results, often leading to the use of harmful organic solvents for extraction. Therefore, in this study, a novel DES-based shaking-assisted extraction procedure for the separation of polyphenolic compounds from plant samples followed by LC-ESI-QTOF-MS analysis was developed. The DES was prepared from choline chloride (ChCl) as the hydrogen bond acceptor (HBA) and fructose (Fru) as the hydrogen bond donor (HBD) at various molar ratios with the addition of 30% water to reduce viscosity. Several experimental variables affecting extraction efficiency were studied and optimized using one-variable-at-a-time (OVAT) and confirmed by response surface design (RS). Nearly the same experimental conditions were obtained using both optimization methods and were set as follows: 30mg of sample, 300mg of ChCl:Fru 1:2 DES containing 30%w/w of water, 500rpm shaking speed, 30min extraction time, 10°C extraction temperature. The results were compared with those obtained using conventional solvents, such as ethanol, methanol and water, whereby the DES-based shaking-assisted extraction method showed a higher efficiency than the classical procedures. The greenness of the developed method was compared with the greenness of existing procedures for the extraction of polyphenolic substances from solid plant samples using the complementary green analytical procedure index (ComplexGAPI) approach, while the results for the developed method were better or comparable to the existing ones. In addition, the practicability of the developed procedure was evaluated by application of the blue applicability grade index (BAGI) metric. The developed procedure was applied to the determination of spruce root samples with satisfactory results and has the potential for use in the analysis of similar plant samples.

Optimization of Ultrasonic-Assisted Extraction of Antioxidants in Apple Pomace (var. Belorusskoje malinovoje) Using Response Surface Methodology: Scope and Opportunity to Develop as a Potential Feed Supplement or Feed Ingredient

Apple pomace represents an underexploited source of bioactive compounds. This study examines the optimization of total phenolic content (TPC) and antioxidant extraction yield of apple pomace (variety: Belorusskoje malinovoje) using response surface methodology. The green extraction technique used was ultrasound-assisted extraction, and it was compared with conventional solvent extraction. The impact of extraction time and amplitude of ultrasound-assisted extraction on the yield of polyphenols and antioxidants has been evaluated. Total phenolic content was determined using an established TPC assay. The antioxidant activity of the apple pomace was determined using established assays 2,2-diphenyl-1-picrylhydrazyl (DPPH•) and 2,2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid (ABTS•+). Furthermore, the potential of apple pomace as a feed material was explored by assessing its nutritional composition, vitamins, minerals, fatty acids, and amino acid content. The extraction of antioxidants and phenolic compounds was efficiently optimized using RSM. The optimal conditions for TPC and DPPH• analyses were achieved with an extraction time of 17.5 min and an ultrasound-assisted extraction amplitude of 20%. Optimal conditions for ABTS•+ were 5 min extraction time and 20% amplitude. Conventional and ultrasound-assisted extraction methods yielded comparable results. Moreover, apple pomace exhibits potential as a feed ingredient despite its modest protein content. This study contributes to the utilization of apple pomace by providing additional information on its antioxidant content and nutritional composition, thus contributing to its sustainable utilization in various industries, especially the livestock feed sector.

Analyzing Alkyl Bromide Genotoxic Impurities in Febuxostat Based on Static Headspace Sampling and GC-ECD.

Herein, a sensitive and selective gas chromatography-electron capture detector (GC-ECD) method was developed and validated for the quantification of trace levels of five bromo-containing genotoxic impurities in Febuxostat active pharmaceutical ingredient (API) after headspace sampling (HS). Multivariate experimental designs for the optimization of static headspace parameters were conducted in two stages using fractional factorial design (FFD) and central composite design (CCD). The optimum headspace conditions were 5 min of extraction time and a 120 °C extraction temperature. Baseline separation on the analytes against halogenated solvents was carried out using an Agilent DB-624 (30 m × 0.32 mm I.D., 1.8 μm film thickness) stationary phase under isothermal conditions. The method was validated according to ICH guidelines in terms of specificity, linearity, the limits of detection and quantification, precision and accuracy. The linearity was assessed in the range of 5-150% with respect to the specification limit. The achieved LOD and LOQ values ranged between 0.003 and 0.009 and 0.01 and 0.03 μg mL-1, respectively. The accuracy of the method (expressed as relative recovery) was in the range of 81.5-118.2%, while the precision (repeatability, inter-day) was less than 9.9% in all cases. The validated analytical protocol has been successfully applied to the determination of the impurities in various Febuxostat API batch samples.

Ultrasonic-assisted extraction and UHPLC determination of ascorbic acid, polyphenols, and half-maximum effective concentration in Citrus medica and Ziziphus spina-christi fruits using multivariate experimental design

This study aimed to determine the concentrations of ascorbic acid and polyphenols in fruits and peels of Citrus medica and Ziziphus spina-christi grown in Ethiopia. Conditions of ultrasound-assisted extraction (UAE) and ultra-high-performance liquid chromatography coupled with a diode array detector (HPLC-DAD) were optimized, using a multivariate experimental design. The optimum conditions of UAE were 15 min extraction time at 35 ℃, with 75 % aqueous methanol as solvent, and a fruit powder-to-solvent ratio (m/v) of 1:15. Among the different drying conditions investigated, freeze-drying was found to be appropriate for analyzing ascorbic acid, polyphenols, and antioxidant potential. The overall ranges, across the fruits and peels, of ascorbic acid, total polyphenols, and antioxidant potentials (EC50) obtained were 8.7 ± 1.4–91.2 ± 2.6 mg/100 g, 253.0 ± 6.3–764.1 ± 25.8 mg GAE/100 g and 2.4 ± 0.1–26.1 ± 2.9 mg/mL, respectively. This indicates that the fruits and peels of the studied plants are advantageous as sources of ascorbic acid and polyphenols.

Recovery of uranium from phosphate ore of Iran mine: Part II- solvent extraction of uranium from wet-process phosphoric acid

The current study in laboratory scale was aimed at developing an optimal two-stage extraction process for production of yellow cake from the phosphoric acid solution that was extracted from the Sheikh Habil phosphate rocks in central Iran. To attain an optimized extraction process, different mixtures of D2EHPA + TOPO + TBP were examined. A total extraction cycle including extraction, stripping and yellow cake precipitation was run to realistically evaluate the performances of the selected mixtures-conditions. As for optimization of the operational conditions, we exploited central composite design (CCD) method, that is a branch of the surface response methodology (RSM), and analyzed the results with standard statistical methods. The O/A (organic to aqueous ratio) = 2, 11 min extraction time, 5 wt% TOPO concentration, 10–15 wt% TBP concentration, 20 wt% D2EHPA concentration, 800 mv oxidation-reduction potential, and 25 °C temperature were obtained as optimum extraction parameters. The O/A = 15, 11 min stripping time, 50 wt% phosphoric acid concentration, 250 mv oxidation-reduction potential, and 40 °C temperature were obtained as optimum stripping parameters. Finally on the last uranium extraction from the H3PO4 strippant on the optimum conditions, the concentration of uranium was more than 4500 ppm with extraction efficiency near to 90 %. Scrubbing of organic phase was done by 2 wt% of sulfuric acid solution at 40 °C and precipitation of ammonium uranyl carbonate (AUC, (NH4)4UO2(CO3)3) was done with 2 M ammonium carbonate solution at an O/A ratio of 1/2 with efficiency more than 95 % in the uranium precipitation process.

Deep Eutectic Solvents as New Extraction Media for Flavonoids in Mung Bean.

Mung beans contain abundant flavonoids like vitexin and isovitexin, which contribute to their strong bioactivities, such as antioxidant effects, so efforts should focus on extracting bioactive flavonoids as well as aligning with the goal of green extraction for specific applications. Deep eutectic solvent coupled with ultrasound-assisted extraction (DES-UAE) was applied to extract flavonoids from mung beans, and eight different DESs were compared on the extraction yield. In addition, the traditional extraction method with 30% ethanol was performed as the reference. The results showed that ethylene glycol-glycolic acid achieved the highest yield among all the DESs, 1.6 times that of the reference values. Furthermore, the DES-UAE parameters were optimized as a 60 mL/g liquid-solid ratio, 30% water content in DES, 200 W ultrasonic power, 67 °C ultrasonic temperature, and 10 min extraction time, leading to the DES extract with the maximum extraction yield of 2339.45 ± 42.98 μg/g, and the significantly stronger DPPH and ABTS radical scavenging ability than the traditional extract. Therefore, employing DES and ultrasonic extraction together offers a green method for extracting flavonoids from mung beans, advancing the development and utilization of plant-derived effective components in a sustainable manner.