Optimal Extraction Conditions Research Articles

B-286 Single Experiment, Single Plate Solid Phase Extraction (SPE) Optimization using 47 Drug Analytes as an Example

Abstract Background SPE of biological matrices isolates analytes of interest from interfering matrix components that can affect LC-MS/MS quantitation. Optimal SPE conditions are dependent upon the sample matrix and analyte properties and typically require multiple experiments to determine optimal conditions for SPE extraction. Here, a 96-well method development plate was utilized to streamline method development for a panel of 47 clinical research drug analytes: 14 antipsychotics, 22 antidepressants and 11 anticonvulsants. Methods An SPE plate with four polymeric sorbents: reversed phase (X), strong and weak cation-exchange and weak anion-exchange mixed-mode phases (X-C, X-CW and X-AW) was used. The 47 drugs analytes were extracted on all four sorbents using three sets of conditions: acidic pretreatment/wash (aq) with basic elution (AB), neutral pretreatment/wash (aq) with neutral elution (NN), and basic pretreatment/wash (aq) with acidic elution (BA). A 50/50 methanol/water wash was also included. Elution used neutral or pH adjusted ethyl acetate/isopropanol or methanol/acetonitrile. A reagent blank, matrix blank, extracted serum samples spiked post-elution (n=2), and spiked serum (n=4) were extracted on each sorbent using each set of conditions. Optimal conditions were determined by calculating absolute percent recovery for each analyte. Results Recovery for antipsychotics was 85-97% using X-CW-AB, except Chlorpromazine (59%). It had better recovery (80%) using X-AB. Recovery for the antidepressants was 75-112% using X-C-AB, except Bupropion (35%) and Selegiline (10%). Bupropion had better recovery (83% and 95%) using X or X-CW and BA. Selegiline had better recovery using X, X-CW and X-AW with BA (83-92%). Anticonvulsants comprise zwitterionic, sulfonamides, neutral, acidic, and basic compounds with widely varying pKa and polarity. Targeting a single method for these analytes is difficult. The best recovery for anticonvulsants used X-CW-AB with several exceptions. Lacosamide, Felbamate, and Levetiracetam are neutral and among the most polar analytes and had 7-31% recovery under all SPE conditions tested. Zwitterionic Gabapentin and Pregabalin had 50-53% recovery from X-CW and X-C sorbents. The stronger protic elution (ammoniated methanol/acetonitrile vs ethyl acetate/isopropanol ) improved solubility for complete elution. Oxcarbazepine had 37% recovery from X-CW-AB, but recovery was 71% under BA conditions. Neutral, polar Zonisamide and Topiramate (Sulfonamide compounds) recovery was 25-26% using X-CW-AB. However, recovery was better (47% and 83%) under NN conditions, suggesting the analytes didn’t undergo complete elution from the X-CW sorbent. A stronger elution solvent would improve recovery from X-CW. Conclusions Most antipsychotics were recovered with X-CW-AB. Most antidepressants could be extracted using X-C-AB. Some analytes had higher recovery using hydrophobic interaction (X) SPE. A single mixed-mode SPE two-step elution protocol using a stronger elution solvent may be feasible. Anticonvulsants had mixed results. Some would require a stronger elution solvent. Some could be included in the other two panels to maximize recovery, but some had low recovery under all conditions tested. The method development plate screened 12 SPE methods for 47 analytes in a single experiment, greatly reducing the time and labor required to identify the best sorbent and starting conditions for SPE extraction optimization for drug analysis. This workflow could be implemented for other SPE method development projects.

Supercritical carbon dioxide chelation extraction of heavy metal ions from drilling fluid waste: Experiment and simulation

This study evaluates the application of supercritical carbon dioxide chelation extraction technology for treating heavy metal ions (Zn2+ and Cr3+) in drilling fluid waste. Through a combination of experimental and molecular dynamics simulation methods, the influence of extraction parameters (temperature, pressure, duration, and chelating agents) on the extraction efficiency are investigated. Findings show that increased duration and pressure significantly improve extraction efficiency, while temperature has a complex effect, initially increasing efficiency but plateauing and slightly decreasing at higher temperatures. The optimum extraction condition with pressure of 220 bar, temperature 348.15 K and an extraction duration of 70 min using ethylene diamine tetraacetic acid (EDTA) as the chelating agent has been determined. Importantly, molecular simulation analysis revealed that citric acid outperforms EDTA in terms of Zn2+ and Cr3+ aggregation by forming larger aggregates with greater numbers of molecules while reducing overall aggregate count. Furthermore, optimization of extraction pressure in the EDTA system shows potential benefits. These results suggest that supercritical carbon dioxide chelation extraction technology has strong potential for environmentally friendly and reliable waste management in the drilling industry. This study represents a significant step forward in developing sustainable solutions for heavy metal removal from drilling fluid waste.

Enzymatic production, physicochemical characterization, and prebiotic potential of pectin oligosaccharides from pisco grape pomace

The prebiotic capacity of Pectin Oligosaccharides (POS) is influenced by structural factors such as molecular size, composition, and degree of esterification, which affect their interaction with the gut microbiota. While existing literature has predominantly examined POS derived from apple and citrus pectins, the extrapolation of these findings to other pectin sources remains complex due to variations in their composition. This study focused on obtaining POS with prebiotic potential from pisco grape pomace through controlled enzymatic hydrolysis, resulting in three molecular size fractions: <3 kDa, 3–10 kDa, and > 10 kDa. The POS fractions were analyzed using FTIR, HPSEC, HPLC, and MALDI-TOF-MS techniques to characterize their physical-chemical properties. Each fraction presented distinct compositions, with the <3 kDa fraction showing a higher concentration of galacturonic acid and glucose, while the >10 kDa fraction was also composed of rhamnose and arabinose. Notably, the <3 kDa fraction supported greater biomass growth of the probiotic strain Lactobacillus casei ATCC 393 compared to the other fractions. In contrast, the non-probiotic strain Escherichia coli ATCC 25922 achieved the lowest biomass with this fraction. Consequently, the <3 kDa POS fraction exhibited the highest prebiotic index. This fraction, composed of oligomers from the rhamnogalacturonan region and arabino-oligosaccharides with a degree of polymerization between two and five, highlights its potential for further research and applications. Therefore, investigating other sources and optimizing extraction conditions could lead to developing novel prebiotic formulations that supply specific probiotic strains for a symbiotic product.

Determination of three dechloranes in environmental water by magnetic solid-phase extraction-gas chromatography-negative chemical ionization mass spectrometry based on the covalent organic framework material

Dechloranes are additive-type chlorine flame retardants that are widely used in processing industrial products, such as electronic equipment and textiles. Dechloranes, which can enter the human body through various routes, pose significant health risks because of their toxicity, persistence, and bioaccumulation. In 2023, dechlorane plus was listed in the Stockholm Convention on Persistent Organic Pollutants. In the same year, China recognized this compound as a priority-controlled substance. Dechloranes are commonly found at trace levels in water, which is extremely harmful to the environment and human health. Therefore, the development of detection methods for dechloranes is crucial. Magnetic solid-phase extraction (MSPE) has attracted considerable attention because of its low organic solvent consumption, simplicity of adsorbent separation, and ease of operation. In general, the selectivity and efficiency of MSPE depend on the characteristics of the adsorbent. Covalent organic frameworks (COFs) have regular porosity, structural predictability and stability, high specific surface areas, and adjustable pore sizes, which are advantageous for a wide range of separation and analysis applications. In this study, Fe3O4 magnetic nanoparticles and a COF material (TpBD) were combined to prepare Fe3O4@TpBD as an adsorbent for dechloranes. Subsequently, an effective method for analyzing dechlorane in environmental water was established by coupling MSPE with gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS). The successful synthesis of Fe3O4@TpBD was confirmed using transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, and vibrating sample magnetometry. A single-factor method was used to optimize the extraction conditions, including the Fe3O4@TpBD dosage, pH of water sample, elution solvent type and volume, extraction time, elution time, and ionic strength. The target analytes were separated on a TG-5SILMS column (30 m×0.25 mm×0.25 μm) and quantified using the external standard method in the selected-ion monitoring (SIM) mode. Under the optimal extraction conditions, the method validation results showed a linear range of 2-1000 ng/L. The limits of detection (LODs) and quantification (LOQs) were 0.18-0.27 ng/L and 0.60-0.92 ng/L, respectively, for the three analytes. The intra-day and inter-day precisions at three spiked levels were 4.2%-16.2% and 6.9%-15.7%, respectively. This method was successfully applied to the determination of dechloranes in environmental water samples (laboratory tap water, reservoir water, wastewater treatment plant effluent, and landfill leachate treatment effluent). The recoveries of the three dechloranes at different spiked levels ranged from 77.8% to 113.3% with relative standard deviations (RSDs) of 2.5%-16.3% (n=3). With the advantages of operational simplicity, high sensitivity, and good reproducibility, the proposed method is suitable for the qualitative and quantitative determination of dechloranes in environmental water.

Sustainable ferritin from bovine by-product liver as a potential resource: Ultrasound assisted extraction and physicochemical, structural, functional, and stable analysis

Ferritin is an iron-containing protein that is widely present in all organisms and has the function of regulating the metabolic balance of iron in organisms. It can be separated from animal by-product tissues and converted into value-added components to promote the development of a circular economy. This study established a method for extracting bovine liver ferritin (BLFer) using ultrasound-assisted buffer system. The optimal extraction conditions were determined through single factor and response surface optimization experiments as follows: ultrasound temperature of 70 °C, extraction time of 25 min, ultrasonic power of 400 W and solvent-to-solid ratio of 2 mL/g, the experimental value of the ferritin yield was 32.18 ± 0.12 g/kg. Compared with traditional methods, Ultrasound-assisted extraction improved the ferritin yield and enhanced its structural stability. Bioinformatics analysis revealed that BLFer is a hydrophilic protein with strong thermal stability. The BLFer has a ferrous oxidase active center, which plays an important role in the oxidative precipitation and reductive release of iron. It can dissociate under strong acids or bases but maintains good stability after heat treatment. These findings will help improve the comprehensive utilization of animal by-products, and promote the potential application of animal by-product ferritin in food and other industries.

Subcritical water extraction on phenolic, flavonoid and antioxidant activity from Orthosiphon Stamineus leaves: Experimental and optimization

Orthosiphon stamineus is rich in phenolic and flavonoid compounds, contributing to its antioxidant properties. This study focuses optimizes the extraction of bioactive compounds from Orthosiphon stamineus leaves using subcritical water (SCW) extraction. Response surface methodology was employed, with temperature (120–180 °C), flow rate (2–8 mL min−1), and extraction time (5–15 min) as independent variables. Dependent variables included extract yield, total phenolic compounds (TPC), total flavonoid compounds (TFC), and antioxidant activity (AA). Optimal conditions were found at 148 °C, 5.1 mL min−1, and 10.5 min, resulting in a maximum yield of 317.6 mg g−1, TPC of 12.71 mg 100 g−1, TFC of 74.09 mg 100 g−1, and AA of 87.48 %. The research highlights the significant influence of temperature as the most crucial parameter, followed by flow rate and extraction time, in achieving the highest yield and bioactive compound content. This investigation holds potential implications for the food processing industry, showcasing the relevance of optimizing extraction conditions to enhance the nutritional and functional properties of natural ingredients like Orthosiphon stamineus in food products.

Optimization of adenosine và cordycepin extraction from cordyceps

Adenosine and cordycepin are bioactive compounds with health benefits. Therefore, both substances are often used to assess the quality of Cordyceps products. The optimization of the extraction conditions to determine adenosine and cordycepin from products containing Cordyceps (powder, extract, and capsule samples) were studied. The samples were prepared using an ultrasound-assisted extraction, the solvent was methanol and quantification of adenosine and cordycepin by HPLC-PDA. Optimization of adenosine and cordycepin extraction conditions by Response surface methodology using the Box-Behnken design, and by using design expert software. The experimental matrix includes 17 experiments of 3 investigation factors with the running range: material/solvent ratio (1:10-1:50 g/mL), methanol concentration (5-25%), ultrasound time (30-90 minutes). The results showed the optimal conditions for the extraction of adenosine and cordycepin for Cordyceps powder samples are the ratio of raw materials:solvent = 1:40 (g/mL), methanol concentration of 17.5% and ultrasound time is 70 minutes, the mean contents of adenosine and cordycepin were 24.15 and 330.78 mg/100g, the optimal methanol concentration for the extraction process is 15% for Cordyceps extract samples, those in their were: 158.30 and 1050.78 mg/100g, the most appropriate methanol concentration is 50% for Cordyceps capsule samples, while those in their were: 23.98 mg/100g and 213.21 mg/100g, relatively. This study provides an efficient analysis method to determine the optimal extraction conditions of adenosine and cordycepin from products containing Cordyceps that can be used as a basis for evaluating the quality of these products.

Optimization of Ultrasonic-Assisted Extraction, Characterization and Antioxidant and Immunoregulatory Activities of Arthrospira platensis Polysaccharides

This study aimed to enhance the ultrasonic-assisted extraction (UAE) yield of seawater Arthrospira platensis polysaccharides (APPs) and investigate its structural characteristics and bioactivities. The optimization of UAE achieved a maximum crude polysaccharides yield of 14.78%. The optimal extraction conditions were a liquid–solid ratio of 30.00 mL/g, extraction temperature of 81 °C, ultrasonic power at 92 W and extraction time at 30 min. After purification through cellulose DEAE-52 and Sephadex G-100 columns, two polysaccharide elutions (APP-1 and APP-2) were obtained. APP-2 had stronger antioxidant and immunoregulatory activities than APP-1, thus the characterization of APP-2 was conducted. APP-2 was an acidic polysaccharide consisting of rhamnose, glucose, mannose and glucuronic acid at a ratio of 1.00:24.21:7.63:1.53. It possessed a molecular weight of 72.48 kDa. Additionally, APP-2 had linear and irregular spherical particles and amorphous structures, which contained pyranoid polysaccharides with alpha/beta glycosidic bonds. These findings offered the foundation for APP-2 as an antioxidant and immunomodulator applied in the food, pharmaceutical and cosmetic industries.

Extraction Condition Optimization, Quantitative Analysis, and Anti-AD Bioactivity Evaluation of Acorn Polyphenols from Quercus variabilis, Quercus aliena, and Quercus dentata

In the present study, Quercus variabilis (Q. variabilis), Quercus aliena (Q. aliena), and Quercus dentata (Q. dentata) acorn kernels were taken as the research objects, and the free polyphenols and bound polyphenols in acorn kernels were extracted using improved ultrasound-assisted ethanolic and alkaline extraction methods, after which the contents of gallic acid, quercetin, azelaic acid, ellagic acid, and ferulic acid were quantified by LC-MC/MS. The results demonstrated that Q. variabilis and Q. aliena acorns were suitable as raw materials to extract ellagic acid, the contents of ferulic acid and bound gallic acid in them were different, and Q. aliena acorns were more suitable for the research of gallic acid, but not for azelaic acid. Results on APP/PS1 transgenic mice verified that five polyphenols significantly suppressed the progression of AD. This study provides a theoretical basis for the drug development of acorn polyphenols.

Determination of Polyphenols in Cigar Tobacco by HPLC

A high performance liquid chromatography (HPLC) method was developed for the determination of neochlorogenic acid, cryptochlorogenic acid and caffeic acid in cigar tobacco. Firstly, the extraction method, extraction liquid concentration and dosage, column temperature and mobile phase flow rate of polyphenols in cigar tobacco were discussed. Then the detection limit, recovery rate, precision and standard curve of three polyphenols were tested. Finally, tobacco samples were tested. The results showed that the optimal extraction conditions were: ultrasonic extraction, extraction time was 30 min, methanol volume concentration was 50%, dosage was 20 mL, the optimal detection conditions were: column temperature was 30 ℃, flow rate was 1.0 mL/min, detection wavelength was 340 nm. The contents of neochlorogenic acid, cryptochlorogenic acid and caffeic acid were in the range of 0~0.202 mg/g, 0~0.331 mg/g and 0.050~0.073 mg/g, respectively, and the linear correlation coefficients of the three polyphenols were ≥0.9991, indicating that the linear correlation of the method was good, and the detection limit was ≤0.066 mg/L. The precision was ≤0.427%, and the recovery was 95.13~96.39%. The results showed that the method had good precision, high accuracy, short analysis time and high detection efficiency, and could be used as an effective method for the detection of polyphenols in cigar tobacco leaves.

Enhancing antioxidant yield from carob (Ceratonia siliqua L.): evaluating the efficacy of maceration and ultrasound-assisted methods

ABSTRACT Our study aimed to optimize carob antioxidant extraction for use in the food, cosmetic, and pharmaceutical industries. Maceration investigated ethanol concentration, extraction temperature, and time, while ultrasound-assisted extraction examined ethanol concentration, ultrasound power, and time. A central composite design with 19 experimental points assessed the influence of variables on total yield, total phenolic content, and antioxidant activity. The results were analyzed to optimize the extraction parameters and enhance the antioxidant extraction from carob. The results of the study show that the best maceration condition for extracting antioxidants from the plant material was found to have a time of 24.38 minutes, an ethanol content of 59.02%, and a temperature of 54.52°C. Similarly, the optimal conditions for ultrasound-assisted extraction were found to be 51.49 minutes, 79.78% sonication power, and 76.12% alcohol. The optimal conditions identified can be used as a starting point for further optimization and scaling up of the extraction process.

Natural deep eutectic solvent-based dispersive liquid-liquid microextraction of pesticides in drinking waters combined with GC-MS/MS detection

The current research aims to develop a new analytical method applying a dispersive liquid-liquid microextraction (DLLME) assisted by vortex and using an environmentally friendly extractant for the preconcentration of organochlorine and organophosphorus pesticides followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. The extractant (i.e., natural deep eutectic solvent (NADES)) is safe, cheap, biodegradable and can be prepared by simply mixing DL-menthol and decanoic acid (molar ratio 2:1). The main experimental factors affecting the extraction of all analytes evaluated (19 organochlorine and organophosphorus pesticides) have been optimised using a multivariate analysis consisting in two steps: a Plackett-Burman design followed by a central composite design (CCD). Seven experimental factors have been evaluated: (i) sample volume; (ii) NADES volume; (iii) sample pH; (iv) extraction time; (v) centrifugation time; (vi) centrifugation speed; and (vii) ionic strength (NaCl %, w v−1). For the significant variables, the optimum values were 10 mL sample and 45 μL NADES. No pH adjustment as well as addition of NaCl were needed. The other variables were set at 3 min extraction time, 5 min centrifugation time and 900×g centrifugation speed, respectively. Under the optimised extraction conditions, the limit of quantification (LOQ) values ranged between 0.2 and 78 ng L−1 for all analysed pesticides. Furthermore, the proposed analytical method has been successfully applied to drinking water (bottled spring water). The recovery study (n = 3) has been evaluated at 0.1, 1.0 and 5.0 μg L−1 spiking levels, obtaining relative recovery values within the range of 70 % and 117 % and RSD values between 1 % and 20 % for all the analytes studied, except for p,p-DDT (56–77 % in high conductivity water samples).

Lithium recovery from an alumina electrolysis slag leaching solution with strong acidity: Separation of lithium-ion and production of battery grade lithium carbonate

Lithium (Li) with excellent physicochemical properties is widely used in modern industries. However, the shortage and depletion of Li resources has hindered the sustainable economic development. Li recovery from waste resource was an effective approach, in particular, alumina electrolysis slag is exemplified as Li riched solid waste. In this work, separation of Li from alumina electrolysis slag leaching solution (AESLS) via solvent extraction using bis(2-ethylhexyl) hydrogen phosphate (P204) system was explored. Effects of saponification degree, phase ratio, and reaction time on metal ions impurities and Li extraction were investigated. Operational parameters including extraction, scrubbing, saponification and precipitation were optimized. Results showed that the extraction efficiencies of Mg2+, Ca2+, Al3+, Fe3+ and Li+ were 100 %, 100 %, 99.99 %, 100 % and 20.71 %, respectively, under the optimal single extraction conditions. The loss of Li after scrubbing of loaded organic phase using hydrochloric acid was as low as 1.59 %. The P204 extraction process was proved to be a thermodynamic process with spontaneous entropy increase, and the extraction order of metal ions was Al3+ > Fe3+ > Ca2+ > Mg2+ > Li+ according to the extraction driving force (ΔC); The solvent-extracted ligand mechanism was elucidated by infrared spectroscopy and nuclear magnetic resonance. Additionally, battery-grade lithium carbonate was produced. Our study paves a new way for recovery of Li in AESLS.

Polysaccharides from Inonotus obliquus employing subcritical water extraction: Extraction optimization, physiochemical properties and bioactivities analysis

As one of the main components in Inonotus obliquus, polysaccharides was potentially to be developed for the special physiochemical properties and bioactivity. However, the low extraction efficiency of Inonotus obliquus polysaccharides (IOP) significantly hindered the in-depth research and development. To achieve a higher extraction yield of IOP, subcritical water was selected and optimized by Box-Behnken Design (BBD) with a more reasonable yield investigation method in the present study. In addition, for the comparative analysis, the physiochemical properties and bioactivity of the subcritical water extracted polysaccharides (IOP-S), purified polysaccharides (IOP-P) and hot water extracted polysaccharides (IOP-W) were all investigated and analyzed. The results showed that the optimal extraction conditions were 200°C, 13.24 min and 30:1 (mL/g), which corresponded to a polysaccharide yield of 14.14±0.17 %. With simple purified process, the IOP-P with high purity (total sugar content of 87.55 %) was suitable for the further study. Compared to IOP-W, a wider molecular weight range (3.4–98 kDa) of polysaccharide was found in IOP-S, as well as higher sugar and polyphenol content, which might be the main reason for the well antioxidant and digestion enzyme inhibition activity. There were also various differences in the monosaccharide composition, micro-morphology and other physiochemical properties, which all suggested that the subcritical water could efficiently extract a special IOP for the fourthly study and development. In summary, the present study proved that subcritical water extraction could significantly improve the extraction efficiency of IOP, and the basic information in physiochemical properties and bioactivities of IOP would promote the development of IOP in the future.

Natural deep eutectic solvents for efficient recovery of bioactive compounds from by-product of industrial hemp processing: Pretreatment, modeling and optimization

Hempseed hull, an underutilized by-product of the hemp processing industry, is a valuable bio-based material. This study aims to optimize phenolic compound extraction by natural deep eutectic solvents (NADES) with enhanced antioxidant properties (DPPH, FRAP, ABTS). By utilizing a chemometric approach, the research was conducted in three stages: selecting high-extractability NADES, identifying crucial extraction variables via screening, and optimizing conditions using response surface methodology (RSM). Fractional factorial experimental design was employed to identify the important variables, while a face-centered central composite experimental design (CCD) was utilized in combination with response surface methodology (RSM) to determine the optimal extraction conditions. The optimal conditions were found using NADES based on L-proline and lactic acid (1:2 ratio) at 39°C for the liquid-solid ratio, 70°C for temperature, and 135 minutes for extraction time. By optimizing extraction conditions this study contributes to advancing our understanding of hempseed hulls' biochemical composition and its potential as bio-based material.

Extraction of polyphenols from Apocynum venetum leaves using customized deep eutectic solvents: Process optimization and antioxidant evaluation

To encourage the commercial utilization of A. venetum polyphenols as bio-colorant on textile, five different combinations of deep eutectic solvents (DESs) were evaluated using a single-factor approach and the extraction of polyphenols from A. venetum leaves by ultrasound-assisted DESs was optimized. At the same time, the antioxidant activity of polyphenols prepared were investigated. The DESs composed of choline chloride and glycerol with a molar ratio of 1:2 and a water content of 20 % showed higher extraction performance than other DESs and traditional solvents (water, 60 % ethanol and 60 % methanol). With the most effective solvent the maximum yield 8.24 % of polyphenols was obtained under the optimal extraction conditions were as follows: the ratio of liquid volume (mL) to solid mass (g) is 49:1, extraction temperature of 77 ℃, and extraction time of 55 min. In addition, the polyphenols that have been separated and purified from the DESs extract exhibited antioxidant activities in three kinds of assays including 2,2-diphenyl-1-picrylhydrazyl stable free radical (DPPH), 2,2’-azino-bis-(3-ethylbenzothiazoline-6-sulfonic) acid free radicals (ABTS) and hydroxyl radical (•OH) scavenging activity. Therefore, this paper demonstrates that DESs are effective and environmentally friendly solvents extraction of antioxidant polyphenols pigments from the leaves of A. venetum.

Optimization and evaluation of biologically active compound with antibacterial and anti-inflammatory properties from peony seed meal

Peony seed meal is produced annually on a large scale in China, resulting in considerable solid residue. Unfortunately, most of this residue is discarded, thereby creating environmental pressure. However, the untapped medicinal value of peony seed meal prompted us to establish an efficient methodology for optimizing the extraction and purification of total alkaloid, followed by a detailed analysis of its biological activities. A single-factor experiment and an orthogonal test were used to identify the optimal extraction parameters. Then, further optimization was performed using the response surface methodology. The extract was enriched using D-101 macroporous adsorption resin. Subsequently, silica gel column chromatography was used for separation, and high-performance liquid chromatography was used for further separation and quantification. Meanwhile, gas chromatography–mass spectrometry (GC–MS) was used to identify alkaloid components. Finally, the antibacterial and anti-inflammatory were evaluated. The optimal extraction conditions substantially improved the yield of alkaloids. A total of 15 alkaloids were separated. GC–MS analysis revealed the presence of Sophoridine, which accounted for 91.88 % of the total alkaloid content. The antibacterial activity of the total alkaloid was tested, and the lowest inhibitory concentrations of E. coli ATCC 25922 and S. aureus ATCC 29213 were 0.04516 and 0.05645 mg/mL, respectively. Additionally, total alkaloid had an inhibitory effect on ear swelling induced by xylene and toe swelling induced by egg white, reducing by 80 % and 24 %, respectively. The current research discovered the antibacterial activity of PSM alkaloid, which has important practical significance for the research and development of new plant-derived antibacterial agents.

Fabrication of a 3D Printer Filamnet Extruder

3D printing, an additive manufacturing process, transforms digital designs into physical objects by layering material. This mechanization adds consecutive layers to build up the complete entity, resulting in a 3D object. It develops objects progressively to formulate the preferred look. Filaments are the main component in a die cast model (FDM) 3D printer, these are thermoplastic substances that are injected through a hot die to form the object. These filaments are available in different types such as PLA, ABS, PETG, HDPE each of which has specific characteristics that offer different applications and material options in 3D printing. This paper depicts about fabricating and developing a design of a 3D filament extruder that can produce 1.75 mm diameter filaments from recycled HDPE material. The extruder consists of a motor, a speed controller, a cylinder, a hopper, band heaters, a thermocouple, a temperature controller, a fan, a nozzle and a winder. This system works in the correct temperature range of 350-370 degrees Celsius for melting thermoplastic materials (recycled HDPE). Extruder function is to feed the material from the nozzle into the hot cylinder. A motor screw pushes the metal into the nozzle, where it becomes the filament. This filament is then injected onto a substrate for later use in 3D printing. The temperature is determined using thermocouples and a temperature controller, which ensures optimal extraction conditions. A fan is designed to quickly cool the removed filament. The objective of this research is to create an economical as well as efficient filament to produce high quality filaments. Extruder performance is evaluated based on filament diameter consistency, material penetration and energy efficiency.

The Testing Results of ACORGA, LIX Extractants and CR60 Crud Mitigation Reagent Influence during SX-EW Copper Extraction

Research analysis reveals factors influencing third-phase crud formation and composition during metal extraction, including solution composition, solid suspensions, organic compounds, colloidal compounds (e.g., silicic acid), and extractant purity. Compositional analysis of copper-containing sulfuric acid solutions (1.25 g/dm3 copper) identifies principal sulfate-forming components. Copper extraction was studied using extractants LIX 984N, ACORGA M5774, and M5640 at different ratios of the organic phase to the aqueous O:A (from 1:2 to 1:10). Suppressive impact of 10 vol.% CR60 additive on third-phase crud formation during copper extraction with LIX 984N, ACORGA M5774, and M5640 is analyzed, with ACORGA M5774 being the most effective. Physicochemical analysis characterizes CR60’s active substance as poly(sodium 4-styrenesulfonate) with steel-suppression properties, and its structural formula is determined. Optimal copper extraction conditions establish ACORGA M5640’s 24% efficiency, followed by ACORGA M5774 at 15%. CR60 reduces crud formation, with 5 cm3 of ACORGA CR60 added to sulfuric acid solution reducing interfacial crud formation by 2–3 times. Optimal extraction parameters include 1:2 O:A ratio, 20 ± 5 °C temperature, 5 cm3 CR60 additive, 5 min process duration, and 1-day settling time. ACORGA M5774 (10 vol.% in kerosene) is recommended as an extractant, with 2–3 stages of countercurrent extraction.

Investigating the potential of aqueous enzymatic extraction of safflower (Carthamus tinctorius L.) seed oil: Process optimization and oil characterization

Safflower seed oil was extracted by aqueous enzymatic extraction (AEE) with a combination of three enzymes: hemicellulase, pectinase, and protease. A Response Surface Methodology (RSM) was performed to optimize the operating conditions: Temperature, pH, and incubation time. Analysis of variance allowed studying the variables' linear, quadratic, and interaction effects. The optimized extraction conditions resulted in 85% oil recovery referring to the conventional Soxhlet extraction (SE). Subsequently, a comparative analysis was conducted to evaluate the quality and composition of oils obtained by SE and AEE. The results revealed that the two oils had similar values of peroxide index, conjugated dienes and trienes, and fatty acid composition. AEE-oil had a lighter yellow color (L* = 31.8 Vs. 24.7) and was richer in polyphenols (147 Vs. 101 mg GAE/Kg of oil), but it was more acidic (2.75% Vs. 1.56% linoleic acid) and less stable (2.86h Vs. 5.66h induction time) with less tocopherol (302 Vs. 409 mg/kg oil) and carotenoid content (0.42 Vs. 0.57 mg/kg oil) than SE-oil. Our findings demonstrated that RSM-based optimization is an efficient and time-saving approach, which significantly improved oil extraction. Finally, we suggested several solutions to further improve the quality and quantity of the obtained AEE-safflower seed oil, paving the path for other future research possibilities.