Optimization Of Extraction Process Research Articles

Alginate Formulation for Wound Healing Applications.

Significance: Alginate, sourced from seaweed, holds significant importance in industrial and biomedical domains due to its versatile properties. Its chemical composition, primarily comprising β-D-mannuronic acid and α-L-guluronic acid, governs its physical and biological attributes. This polysaccharide, extracted from brown algae and bacteria, offers diverse compositions impacting key factors such as molecular weight, flexibility, solubility, and stability. Recent Advances: Commercial extraction methods yield soluble sodium alginate essential for various biomedical applications. Extraction processes involve chemical treatments converting insoluble alginic acid salts into soluble forms. While biosynthesis pathways in bacteria and algae share similarities, differences in enzyme utilization and product characteristics are noted. Critical Issues: Despite its widespread applicability, challenges persist regarding alginate's stability, biodegradability, and bioactivity. Further understanding of its interactions in complex biological environments and the optimization of extraction and synthesis processes are imperative. Additionally, concerns regarding immune responses to alginate-based implants necessitate thorough investigation. Future Directions: Future research endeavors aim to enhance alginate's stability and bioactivity, facilitating its broader utilization in regenerative medicine and therapeutic interventions. Novel approaches focusing on tailored hydrogel formations, advanced drug delivery systems, and optimized cellular encapsulation techniques hold promise. Continued exploration of alginate's potential in tissue engineering and wound healing, alongside efforts to address critical issues, will drive advancements in biomedical applications.

Optimization of curdlan production and ultrasound assisted extraction processes from Priestia megaterium

In this study, the upstream and downstream production processes of curdlan from Priestia megaterium were optimized to enhance its yield. Additionally, a novel extraction method was developed for curdlan recovery. Optimization studies were conducted using Central composite design (CCD). Curdlan yield improved from 0.15 g/L (unoptimized) to 0.46 g/L (3-fold increase) when fermentation was carried out in CCD-optimized media of (w/v) sucrose 20%, urea 0.1%, KH2PO4 0.02%, agitation speed 250 rpm. To further enhance curdlan yield during extraction, ultrasonication was incorporated as a novel step into the conventional method of acid/alkali-assisted curdlan recovery. A two-step optimization was chosen for extraction, namely, one-factor-at-a-time (OFAT) and CCD, wherein the optimized extraction parameters were determined to be 25 s sonication, 1 N NaOH, and 2 h solubilization time. The curdlan yield improved by 1.5-fold (0.70 g/L) post optimization, in comparison with unoptimized conventional extraction step. Finally, the biopolymer was validated through characterization by nuclear magnetic resonance (NMR) which showed characteristic curdlan spectra in the13C and1H NMR studies. To the best of our knowledge, this study represents the first documented report on curdlan extraction using this novel method of ultrasonication.

Optimization of Extraction Process, Structure Characterization, and Immunomodulatory Activity of Polysaccharides from Black Garlic

AbstractUltrasound assisted extraction (UAE) was used to extract polysaccharides from black garlic, and the extraction process for UAE of black garlic polysaccharides (BGPs) was optimized via RSM coupled with genetic algorithm. The optimal extraction process parameters were obtained as follows: extraction time of 30 min, liquid‐to‐solid ratio of 29 mL/g, extraction temperature of 51 ℃, and ultrasound power of 418 W, and the yield of BGPs was 10.17% ± 0.14%. Subsequently, the crude BGPs were further purified by DEAE‐52 cellulose and Sephadex G‐100 to obtain a homogeneous fraction (BGPs‐1‐SG with the molecular weight of 1.37 × 106 Da) that was comprised of mannose (Man), glucuronic acid (GlcA), rhamnose (Rha), glucose (Glc), and fucose (Fuc) with a molar ratio of 40.23:71.06:2.96:85.38:7.32. Congo red and circular dichroism spectroscopy indicate that BGPs‐1‐SG has a triple helix structure. Scanning electron microscope and atomic force microscope demonstrate that BGPs‐1‐SG showed irregular structures including sheet‐like, rod‐shaped, irregular spherical structures, and aggregated in aqueous solutions. Moreover, BGPs‐1‐SG could increase viability, phagocytic rate, and NO content of RAW264.7 cells. Furthermore, BGPs‐1‐SG could promote the secretion and mRNA expression levels of IL‐1β, IL‐6, and TNF‐α. The findings can provide an important reference for the development of functional foods.

Self‐Driving Lab for Solid‐Phase Extraction Process Optimization and Application to Nucleic Acid Purification

Sorptive bioprocesses are the basis for numerous biotechnological applications such as enzyme immobilization, biosensors, controlled drug delivery, water treatment, and molecular purification. Yet due to the complexity of these processes, their optimization is still time, labor, and cost‐intensive. This research presents a flexible self‐driving laboratory (SDL) designed for the accelerated development and optimization of solid‐phase extraction processes. As a use case, the SDL was used to optimize a DNA purification process using silica magnetic beads. Through the integration of robotics, machine learning, and data‐driven experimentation, the SDL demonstrates a highly accelerated process optimization with minimal human intervention. In the multistep purification approach, the system is able to optimize buffer compositions for DNA extraction from complex samples, demonstrating effectiveness in both conventional chaotropic salt‐based methods and innovative chaotropic salt‐free buffers. The study highlights the SDL's capability to autonomously refine process parameters, achieving significant enhancements in yield and purity of the product. This blueprint for future self‐driving optimization of bioprocess parameters showcases the potential of autonomous systems to revolutionize biochemical process development, offering insights into scalable, environmentally sustainable, and cost‐effective solutions.

Metaheuristic optimized complex-valued dilated recurrent neural network for attack detection in internet of vehicular communications

The Internet of Vehicles (IoV) is a specialized iteration of the Internet of Things (IoT) tailored to facilitate communication and connectivity among vehicles and their environment. It harnesses the power of advanced technologies such as cloud computing, wireless communication, and data analytics to seamlessly exchange real-time data among vehicles, road-side infrastructure, traffic management systems, and other entities. The primary objectives of this real-time data exchange include enhancing road safety, reducing traffic congestion, boosting traffic flow efficiency, and enriching the driving experience. Through the IoV, vehicles can share information about traffic conditions, weather forecasts, road hazards, and other relevant data, fostering smarter, safer, and more efficient transportation networks. Developing, implementing and maintaining sophisticated techniques for detecting attacks present significant challenges and costs, which might limit their deployment, especially in smaller settings or those with constrained resources. To overcome these drawbacks, this article outlines developing an innovative attack detection model for the IoV using advanced deep learning techniques. The model aims to enhance security in vehicular networks by efficiently identifying attacks. Initially, data is collected from online databases and subjected to an optimal feature extraction process. During this phase, the Enhanced Exploitation in Hybrid Leader-based Optimization (EEHLO) method is employed to select the optimal features. These features are utilized by a Complex-Valued Dilated Recurrent Neural Network (CV-DRNN) to detect attacks within vehicle networks accurately. The performance of this novel attack detection model is rigorously evaluated and compared with that of traditional models using a variety of metrics.

Optimization of extraction for efficient recovery of kenaf seed protein isolates: evaluation of physicochemical and techno-functional characteristics.

Kenaf seeds are a rich source of protein; however, finding the best extraction method is crucial to obtaining high-quality protein from these underutilized seeds. This research devised an optimized extraction process for best recovery of kenaf seeds protein using response surface methodology. The key parameters affecting the yield and protein content were optimized, including extraction pH (2-11), seed:water ratio (5:1-50:1), temperature (30-90 °C), and duration (20-360 min). The physicochemical and techno-functional properties of kenaf seed protein isolates (KSPIs) were examined. A maximum protein yield of 12.05 g/100 g with purity level 91.94 g/100 g was obtained using an optimized extraction with pH 11.0, seed:water ratio 50:1, 360 min duration, and temperature 50 °C. The oil and water retention capacities of KSPI were 1.14 mL g-1 and 1.37 mL g-1 respectively. After 30 min at pH 7, KSPIs demonstrated remarkable emulsion capacity (83.12%) and stability (75.63%), along with high foaming capacity (106%) and stability (18.3%). As per high-performance liquid chromatography analysis, arginine, glutamic acid, leucine, phenylalanine, and lysine were the most abundant amino acids detected in KPSIs. The KSPIs' globular protein structure was successfully verified using analytical approaches, including Fourier transform infrared spectroscopy, protein fraction ratios, and differential scanning calorimetry. Sodium dodecyl sulfate polyacrylamide gel electrophoresis analysis revealed that KPSI has a molecular weight distribution ranging from 10 kDa to 50 kDa. The results of this study support the application of the proposed response-surface-methodology-optimized extraction method for efficient recovery of high-quality kenaf seed proteins that meet the necessary physicochemical and techno-functional requirements. © 2024 Society of Chemical Industry.

Optimization of extraction process of polysaccharide from Phylloporia fontanesiae and its simulated digestion in vitro.

In this study, Phylloporia fontanesiae polysaccharide was successfully isolated through a sequential water extraction and alcohol precipitation process. Utilizing the Box-Behnken design, the extraction process was optimized based on single-factor experiments, considering variables such as the material-to-liquid ratio, extraction temperature, extraction time, and the number of extractions. The polysaccharide composition of P. fontanesiae is predominantly composed of mannose, glucuronic acid, glucose, and galactose, with a molar mass ratio of 4.31:4.10:36.83:1, along with minor amounts of aminoglucose and fucose. The polysaccharide fraction of P. fontanesiae comprises two distinct components, possessing relative molecular masses of 8.85kDa and 134.03kDa. Notably, the polysaccharide exhibited significant antioxidant activity. After undergoing simulated gastrointestinal digestion, no significant changes were observed in its antioxidant activity, molecular weight, or monosaccharide composition. This study not only enhanced the extraction efficiency of P. fontanesiae polysaccharide but also provided valuable insights into its composition, structure, and digestion characteristics. PRACTICAL APPLICATION: The optimum extraction process, stability, and antioxidant activity of Phylloporia fontanesiae polysaccharide during simulated digestion of gastrointestinal tract were studied. The results provide a theoretical basis for the development and application of this polysaccharide in the field of food and health products.

Optimization of White Tea Flavanol Extraction Process by the Ultrasonic‐Assisted Deep Eutectic Solvent Method and Determination of the Antioxidant and Antibacterial Activity

ABSTRACTFlavanols have a variety of health benefits and biological activities and become the hotspot of the food development and research. In this research, flavanols were extracted from white tea by ultrasonic‐assisted deep eutectic solvent (DES) method. High‐performance liquid chromatography was used to determine the content of flavanols. The influence of four factors on the flavanol extraction yield was analyzed by single factor experiments, including deep eutectic solvent mole ratio (the mole of hydrogen bond acceptors: the mole of hydrogen bond donors), solid–liquid ratio (white tea sample weight/g: the volume of DES/mL), extraction time and extraction temperature. On the basis of single factor experiments, the factors which had significant effects on the flavanol extraction yield were further optimized by the response surface test. The results showed that the optimized extraction conditions were as follows: the mole ratio of DES 1: 4 (choline chloride: 1,2‐propanediol), the solid–liquid ratio 1:30, the extraction temperature 56°C, the extraction time 53 min, and the ultrasonic power 341 W. Under the above parameters, the extraction yield of white tea flavanols was 9.63 mg/g. After purification with macroporous resin, antioxidation and antibacterial experiments were carried out. The results showed that the antioxidant and antibacterial effects of white tea flavanols were remarkable. The antibacterial effects performed best on Escherichia coli, followed by Bacillus subtilis and Staphylococcus aureus. The maximum diameter of the antibacterial zone on Escherichia coli was 0.95 ± 0.11 mm. The best radical scavenging rates of OH, ABTS+ and DPPH were 97.1%, 97.5%, and 88.4%, respectively, when the flavanol concentration was 9.5 mg/mL. The conclusions of this research can provide theoretical foundation for the further study of white tea flavanols.

Optimization of Sugar Extraction Process from Date Waste Using Full Factorial Design Toward Its Use for New Biotechnological Applications.

In Tunisia, the date industry generates a large quantity of waste, raising environmental concerns. However, dates are rich in sugars, which offer a renewable source of nutrients for various applications. In this study, sugar extraction from two low-grade pitted date fruits (Alig and Kentichi) under ultrasound, was optimized using full factorial design. At 40 °C, for20 min, and with a liquid-to-solid ratio of 10 mL/g, the optimum sugar contents were 60.87% and 50.79% for the varieties Alig and Kentichi, respectively. The date extracts were chemically analyzed, revealing low fat and protein contents, but significant polyphenol and mineral contents in both varieties. HPLC-IR analysis revealed more inverted sugars (glucose and fructose) in the Alig variety and more sucrose in the Kentichi variety. FTIR and SEM analysis showed the efficiency of the ultrasonic treatment of the biomass in terms of improving mass transfer diffusion through ultrasonic cavitation. Thus, ultrasound-assisted extraction constitutes an effective method for the recovery of sugar from date waste.

Natural surfactant used as an additive in the enzymatic-homogenate synergistic extraction of piceatannol, resveratrol, and myricetin from the myrtle (Rhodomyrtus tomentosa) fruit

In this study, three different target analytes from the fruit of myrtle (Rhodomyrtus tomentosa) were extracted via an enzymatic-homogenate synergistic extraction (EHSE) process, and 10 different aqueous solutions of natural surfactants were selected as extraction solvents, thus enabling the simultaneous extraction of piceatannol, resveratrol, and myricetin from the fruit of myrtle (Rhodomyrtus tomentosa). Important factors affecting the yield of piceatannol, resveratrol, and myricetin, including enzyme type, enzyme concentration, pH, surfactant type and dosage, homogenization time, liquid‒solid ratio, incubation and extraction time, incubation time and extraction temperature, were optimized via single-factor experiments. Three important parameters were optimized via the Box‒Behnken design: the liquid‒solid ratio, the incubation–extraction time, and the reaction temperature. The final optimum extraction process conditions were as follows: β-glucosidase concentration, 3.0%, homogenate; time, 3 min; pH, 5; tea saponin concentration, 0.8%; liquid‒solid ratio, 45 mL/g; incubation–extraction time, 2.5 h; and temperature, 67.5 °C. With the optimized experimental parameters, the piceatannol, resveratrol, and myricetin yields were 742.12 ± 37.11 μg/g, 18.58 ± 0.94 μg/g, and 24.83 ± 1.25 μg/g, respectively. Methodological validation and comparison experiments with traditional solvents demonstrated that EHSE is a successful, green, and safe method for extracting active plant components. This approach employs an ecologically benign water-based solution of tea saponin as the extraction solvent, and it combines enzymatic and homogenate procedures to increase extraction efficiency. This study provides a reasonable basis for the application and research of synergistic extraction technology and suggests that more diverse solvent choices should be considered.

Improved yield of UV and heat-stable Monascus yellow pigment by statistical optimization of solid-state fermentation conditions and extraction process

Monascus species are well-known for their ability to produce biocolorants. A high-performing strain, M. purpureus F2–19, was recently developed by genome shuffling. Here, the entire bioprocess, starting from solid-state fermentation conditions to the extraction method, was statistically optimized to improve yellow pigment yield by the strain. Among culture conditions, monosodium glutamate concentration (used as nitrogen source), moisture content, and incubation period significantly influenced pigment production using less expensive broken rice as a substrate. Post-optimization, a yield of 1548.4 ± 14.6 AU/g was achieved, representing a 9.7-fold increase over the primary condition. The statistical model developed using central composite design of response surface methodology (CCD-RSM) is highly significant, with a P value of <0.0001. Similarly, a significant model (P < 0.0001) for extraction improved pigment yield further by 1.16-fold (actual output: 1796.4 ± 13.4 AU/g). The pigment remained highly stable with a preservation rate of ~90 % after 2.5 h exposure to a high temperature of 100 °C or UV light (254 nm). Even autoclaving at 121 °C for 15 min preserved 96.9 % of the pigment. These values are higher than reported for other commercial microbial yellow pigments, riboflavin, β-carotene, or lutein, thus highlighting its potential as a natural food colorant. Liquid chromatography-mass spectrometry (LC-MS) of the pigment identified nine distinct yellow compounds, with monascin being the most abundant. Thus, the optimized bioprocess would facilitate economical large-scale production of the yellow pigment; but its implementation still requires efficient selection of bioreactors and optimizations of scaling-up, especially the heat and mass transfer parameters.

Antidiabetic and Antigout Properties of the Ultrasound-Assisted Extraction of Total Biflavonoids from Selaginella doederleinii Revealed by In Vitro and In Silico Studies.

In this study, the extraction, purification and metabolic enzyme inhibition potential of Selaginella doederleinii were investigated. In order to extract the total biflavonoids from S. doederleinii (SDTBs), the optimum extraction process was obtained by optimizing the ultrasonic extraction parameters using response-surface methodology. This resulted in a total biflavonoid content of 22.26 ± 0.35 mg/g. Purification of the S. doederleinii extract was carried out using octadecylsilane (ODS), and the transfer rate of the SDTBs was 82.12 ± 3.48% under the optimum purification conditions. We determined the effect of the SDTBs on α-glucosidase (AG), α-amylase and xanthine oxidase (XOD) and found that the SDTBs had an extremely potent inhibitory effect on AG, with an IC50 value of 57.46 μg/mL, which was much lower than that of the positive control. Meanwhile, they also showed significant inhibition of XOD and α-amylase, with IC50 values of 289.67 μg/mL and 50.85 μg/mL, respectively. In addition, molecular docking studies were carried out to understand the nature of the action of the biflavonoids on AG and XOD. The results showed that robustaflavone had the lowest binding energy to AG (-11.33 kcal/mol) and XOD (-10.21 kcal/mol), while, on the other hand, amentoflavone showed a good binding affinity to AG (-10.40 kcal/mol) and XOD (-9.962 kcal/mol). Moreover, molecular dynamics simulations verified the above results.

Microfluidic supercritical CO2 applications: Solvent extraction, nanoparticle synthesis, and chemical reaction

Supercritical CO2, known for its non-toxic, non-flammable and abundant properties, is well-perceived as a green alternative to hazardous organic solvents. It has attracted considerable interest in food, pharmaceuticals, chromatography, and catalysis fields. When supercritical CO2 is integrated into microfluidic systems, it offers several advantages compared to conventional macro-scale supercritical reactors. These include optical transparency, small volume, rapid reaction, and precise manipulation of fluids, making microfluidics a versatile tool for process optimization and fundamental studies of extraction and reaction kinetics in supercritical CO2 applications. Moreover, the small length scale of microfluidics allows for the production of uniform nanoparticles with reduced particle size, beneficial for nanomaterial synthesis. In this perspective, we review microfluidic investigations involving supercritical CO2, with a particular focus on three primary applications, namely, solvent extraction, nanoparticle synthesis, and chemical reactions. We provide a summary of the experimental innovations, key mechanisms, and principle findings from these microfluidic studies, aiming to spark further interest. Finally, we conclude this review with some discussion on the future perspectives in this field.

Rapid determination of chlorate and perchlorate in tea by ion exchange chromatography-tandem mass spectrometry

Ion exchange chromatography-tandem mass spectrometry (IEC-MS/MS) has recently become the preferred method for detecting ionic substances in tea. In this study, an IEC-MS/MS method was developed for the rapid determination of chlorate and perchlorate residues in tea samples. The optimal sample extraction process, pretreatment column, and chromatographic and mass spectrometric conditions were systematically investigated. In the optimal process, the tea samples were ultrasonically extracted with methanol-water (13∶7, v/v), and a PRiME HLB SPE column was used to purify the sample extract. An AceChrom Hybri-A IEC column (150 mm×2.1 mm, 5.0 μm) was used for separation, and 100 mmol/L ammonium acetate-acetonitrile (40∶60, v/v) was used as the mobile phase for isocratic elution. The flow rate was 0.3 mL/min, the column temperature was 40 ℃, and the injection volume was 5.0 μL. The mass spectrometric data were collected in negative electrospray ionization mode combined with multiple reaction monitoring (MRM) mode to achieve the rapid and accurate separation and qualitative analysis of the desired chemical components. Quantification was performed using the internal standard (IS) method. The measurement results showed a good linear relationship when the mass concentrations of chlorate and perchlorate were between 2.00-200 and 1.00-100 μg/L, respectively, with correlation coefficients (r2) greater than 0.9990. The average recoveries of chlorate and perchlorate at three spiked levels of low, medium, and high ranged from 88.54% to 97.25% with relative standard deviations (RSDs, n=7) of 3.2%-5.2%. The limits of detection for chlorate and perchlorate were 12.0 and 8.0 μg/kg, respectively, while the limits of quantification were 40.0 and 26.6 μg/kg, respectively. The results of tests conducted to assess the linearity, specificity, accuracy, precision, and applicability of the method to the analysis of chlorate and perchlorate in 15 tea samples collected from a local market demonstrated its validity for the routine analysis of tea samples. The proposed method is simple, rapid, sensitive, and accurate, and can meet requirements for the rapid screening and quantitative analysis of residual trace chlorate and perchlorate in large quantities of tea samples.

Study on Preparation Technology and Quality Standard of Acne Granules

AbstractThe study aimed to optimize the preparation process of acne granules and establish their quality standards. In this work, the extraction process of Chinese herbal extract was optimized by the amount of water added, the number of decoction, the extraction time, and the soaking time with extraction yield as an evaluation index. The indexes of the acne granules such as molding rate, dissolvability, angle of repose, moisture content, and ease of preparation were evaluated. Thin-layer chromatography (TLC) was used to identify Salviae, Scutellaria baicalensis, and Indigowoad Leaf. High-performance liquid chromatography (HPLC) was used to determine the baicalin content in the granules. Based on orthogonal and single-factor experiments, the optimized extraction process of the prescription of nine medicinal materials was as follows: soaked in cold water for 2 hours, boiled three times, decocted with eight times the amount of water for 1.5 hours for the first time, and six times the amount of water for 1 hour for the second and third times. The combined extracts were concentrated to a relative density of 1.30 to 1.40 (20–30°C), and mixed evenly according to the mass ratio of extract to excipient 1:5, and dextrin: powdered sugar = 1:3. The mixture was granulated, dried, prepared into granules, and the acne granules were formed at a molding rate of 95.52% and a critical relative humidity of 82%. The spots in TLC were clear and easy to identify. The HPLC result showed that the content of baicalin was not less than 1.0 mg/g. The study provides a valuable reference for the production and preparation of the granules through optimization of the wet process and the excipient dosage. Furthermore, the established TLC method for the identification and the HPLC method for baicalin quantification laid the foundation for the quality control of the preparation in future studies.

Optimization of the extraction process of total steroids from Phillinus gilvus (Schwein.) Pat. by artificial neural network (ANN)-response surface methodology and identification of extract constituents

Phillinus gilvus (Schwein.) Pat has pharmacological effects such as tonifying the spleen, dispelling dampness, and strengthening the stomach, in which sterol is one of the main compounds of P. gilvus, but there has not been thought you to its extraction and detailed identification of its composition, in the present study, we used artificial neural network (ANN) and response surface methodology (RSM) to optimize the conditions of ultrasonic-assisted extraction, and the parameters of the independent and interaction effects were evaluated. Ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF-MS/MS) was used to identify the major components in the purified extract. The results showed that the optimal extraction process conditions were: ultrasonic time 96 min, ultrasonic power 140 W, liquid to material ratio 1:25 g/ml, and ultrasonic temperature 30.7 °C. The compliance rates of the predicted and experimental values for the artificial neural network model and the response surface model were 98.3% and 96.12%, respectively, indicating that both models have the potential to be used for optimizing the extraction process of P. gilvus in industry. A total of 120 compounds and 30 major steroids were identified by comparison with the reference compounds. Among the major steroidal components are these findings will contribute to the isolation and utilization of active ingredients in P. gilvus.

Optimization and Characterization of PEG Extraction Process for Tartary Buckwheat-Derived Nanoparticles.

Plant-derived edible nanovesicles serve as crucial nanocarriers for targeted delivery of bioactive substances, including miRNAs and phytochemicals, to specific tissues. They have emerged as a significant focus in precision nutrient delivery research. In this study, Tartary-buckwheat-derived nanoparticles (TBDNs) were isolated and purified using a combination of differential centrifugation and PEG precipitation. A response surface test was employed to optimize the extraction process of TBDNs in terms of yield, total phenol and flavonoid content, as well as antioxidant activity. The results demonstrated that TBDNs exhibited the highest yield and activity at a 10% concentration of PEG, pH 5, and centrifugation temperature of 4 °C. Under these conditions, the measured yield of TBDNs was 1.7795 g/kg, with a total phenol content of 178.648 mg/100 g, total flavonoid content of 145.421 mg/100 g, and DPPH-radical-scavenging rate reaching 86.37%. Characterization through a transmission electron microscope and nanoparticle-size-tracking analyzer revealed that TBDNs possessed a teato-type vesicle structure with dispersed vesicle clusters present within them. Furthermore, the extracted TBDNs were found to have an average particle size of 182.8 nm with the main peak observed at 162.8 nm when tested for particle size distribution analysis. These findings provide a novel method for extracting TBDNs while laying the groundwork for future investigations into their activities.

Lab-made automated parallel-dispersive pipette extraction device for the determination of polycyclic aromatic hydrocarbons in distilled beverages (sugarcane spirits) using HPLC-DAD

This work describes the development of a new automated parallel dispersive tip microextraction method (Au-Pa-DPX) for the determination of eleven polycyclic aromatic hydrocarbons (PAHs) in four samples of Brazilian sugarcane spirit beverages, with separation and detection done by the HPLC-DAD. The results obtained with the Au-Pa-DPX approach were also compared with those obtained via the conventional parallel manual DPX method with the same samples and optimized extraction process. Desorption solvent and cycles of desorption, cleaning and extraction were optimized using response surface methodology and univariate approaches. For the Au-Pa-DPX method, the coefficient of determination (R2) ranged from 0.9948 to 0.9997. The limits of detection and quantification were all 0.303 μg l-1 and 1.00 μg l-1, respectively. Interday and intraday precision ranged from 7.6 % to 31.7 % and 0.40 % to 15.8 %, respectively. For the manual parallel DPX method, the interday and intraday precision ranged from 8.2 % to 38.1 % and 5.40 % to 18.7 %, respectively. The relative recovery values obtained with the proposed method ranged from 53.29 to 124.94 %. The enrichment factors ranged from 15.13 to 22.35. The sum of PAH concentrations in the four samples ranged from undetected to 25.58 μg l-1. These results, when correlated to other methods, highlight the gains in regards to precision obtained with the automated apparatus. Furthermore, when compared to other methods from the literature, it is an interesting green alternative for the determination of these analytes and this sample, with high throughput (4.67 min per sample), low consumption of solvents and samples, generating less waste and reducing health risks to the analyst.

Ultrasound-assisted deep eutectic solvents extraction of podophyllotoxins from Juniperus sabina L: Optimization, enrichment, and anti-drug resistant bacteria activity

Podophyllotoxin, along with its congeners and derivatives exhibit strong biological activity mainly as antitumor drugs and antiviral agents. Here, the ultrasound-assisted extraction of podophyllotoxins including α-peltatin, podophyllotoxin, podophyllotoxinone and deoxypodophyllotoxin from Juniperus sabina L. leaves using deep eutectic solvents (DESs) were developed first time. To simultaneously and effectively extract four target podophyllotoxins, 19 DESs were screened to determine the best solvent to extract podophyllotoxins. Choline chloride-lactic acid (1:1) with 30 % water content was proved to have the best extraction effect. The optimal extraction process with DES were DES/solid ratio 30 mL/g, reaction temperature 44℃, time 53 min and ultrasound power 495 W. Under optimized extraction conditions, the total podophyllotoxins extraction yield was 27.520 mg/g, 196.84 % higher than that using traditional methanol solvent. The yield of α-peltatin, podophyllotoxin, deoxypodophyllotoxin and podophyllotoxinone were 13.567, 9.548, 2.021, 2.204 mg/g, respectively. Subsequently, the podophyllotoxins were effectively isolated from the deep eutectic solvent using D101 macroporous resin. The optimal process for enriching target podophyllotoxins by D101 macroporous resin were as follows: 30 mg/mL of crude extract solution, five bed volumes feed volume for adsorption; six bed volumes of 80 % ethanol for desorption. Moreover, a scale-up enrichment experiment of podophyllotoxins was performed under optimum procedure, and the results showed that the target podophyllotoxins yield was increased by 8.92 times, with recoveries in the range of 75.86–85.69 %. Additionally, the enriched podophyllotoxins effectively restored the antibacterial efficacy of cefazolin against methicillin-resistant Staphylococcus aureus and colistin-resistant Escherichia coli, resulting in 16–64-fold reduction in MIC. Therefore, the method developed in this study could be an eco-friendly, efficient and sustainable alternative for the selective extraction and enrichment of active compounds from plant material.

Optimization of Pectin Extraction Process from Albedo of Citrus Lemon (Citrus limon) Using Ultrasonic Method

Abstract Pectin is an industrial raw material that can form gels, thickeners, and emulsifiers widely applied in the food and non-food industries. Extracting pectin with citric acid solvent using ultrasonic waves is considered more effective and efficient. This study aimed to obtain an optimization model for the pectin production process to produce maximum pectin yield and obtain the optimized pectin characteristics. This study used the Response Surface Methodology (RSM) as the optimization method with the Central Composite Design (CCD) experimental design with Design Expert 13 software to determine the treatment combination based on time factors and solvent concentration. The treatment combination obtained was 11. The results showed that the maximum pectin yield value was 34.63% at a 7-minute extraction time using the citric acid solvent concentration of 20% and a validation value accuracy of 99.08%. The optimized pectin characteristics were a water content of 7.66%, ash content of 0.33%, equivalent weight of 183.28 mg, methoxyl content of 7.52%, galacturonic acid content of 67.13%, and degree of esterification of 63.56%. The pectin produced followed the pectin quality standards according to the International Pectin Producers Association (IPPA), except for the equivalent weight. Keywords: extraction, lemon albedo, pectin, ultrasonic Abstrak Pektin merupakan bahan baku industri yang memiliki kemampuan dalam pembentukan gel, zat pengental, dan sebagai zat pengemulsi yang banyak diaplikasikan pada industri pangan dan non-pangan. Proses ekstraksi pektin dengan pelarut asam sitrat menggunakan bantuan gelombang ultrasonik dianggap lebih efektif dan efisien. Tujuan penelitian adalah untuk mendapatkan model optimasi proses produksi pektin hingga menghasilkan rendemen pektin yang maksimum dan mendapatkan karakteristik pektin hasil optimasi. Metode optimasi dalam penelitian ini menggunakan Response Surface Methodology (RSM) dengan dengan rancangan eksperimen Central Composite Design (CCD) menggunakan software Design Expert 13 untuk menentukan kombinasi perlakuan berdasarkan faktor waktu dan konsentrasi pelarut. Kombinasi perlakuan yang diperoleh adalah 11. Hasil penelitian menunjukkan bahwa nilai rendemen pektin maksimum adalah 34,63% pada waktu ekstraksi 7 menit dengan konsentrasi pelarut asam sitrat 20% dengan keakuratan nilai validasi adalah 99,08%. Karakteristik pektin hasil optimasi diperoleh nilai kadar air 7,66%, kadar abu 0,33%, berat ekuivalen 183,28 mg, kadar metoksil 7,52%, kadar asam galakturonat 67,13%, dan derajat esterifikasi 63,56%. Pektin yang dihasilkan sudah sesuai dengan standar mutu pektin menurut International Pectin Producers Association (IPPA) kecuali pada berat ekuivalen. Kata kunci: albedo lemon, ekstraksi, pektin, ultrasonik