Selected Extraction Conditions Research Articles

Polyphenol composition and antioxidant activity of fermentation combined with enzymatic hydrolysis modified Astragalus membranaceus stems

Astragalus membranaceus (AM) roots are a well-known homologous medicine and food in China. AM stems, which are discarded and not used effectively, also contain many active compounds and exhibit beneficial effects. It has the potential to be explored as antibiotic alternative. Fermentation combined with enzymatic hydrolysis (FEH) is an effective strategy for extracting polyphenol and improving the usage of AM stems. Therefore, in this study, the conditions of FEH and extraction for polyphenol in AM stems were screened. The antioxidant activity of extract from AM stems without and with FEH (AMSE and FAMSE) was evaluated. The metabolite profiles of phenolic acids and flavonoids in AMSE and FAMSE were characterized by ultra-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC–ESI-MS/MS). The results showed that the highest polyphenol content from AM stems was obtained with cellulase and pectinase (1:1, 2000 U/g), moisture content 43%, fermentation temperature 30 °C, and fermentation time 7 days. Selected extraction conditions of polyphenol were ethanol concentration 50%, ultrasonic power 500 W, extraction temperature 35 °C, and extraction time 40 min. On this condition, compared with AMSE, the polyphenol and flavonoid contents in FAMSE were significantly higher. FAMSE exhibited stronger DPPH, hydroxyl radical scavenging rate and reducing power than AMSE. The relative content of 3-(4-hydroxyphenyl)-propionic acid, dihydroferulic acid, isoferulic acid, 4-hydroxybenzoic acid, 4-hydroxyphenyllactic acid, ferulic acid, vanillic acid, syringic acid, gentisic acid, sinapic acid, apigenin, tricin, acacetin, daidzein, genistein, formononetin, prunetin, pratensein, rhamnocitrin and galangin were significantly upregulated in FAMSE.Graphical

Rhus microphylla leaves extracts obtained by ohmic heating: Physicochemical composition and bioactive properties

Rhus microphylla Engel. Ex A. Gray is a traditional plant used in folk medicine for various conditions, yet research on its biological potential is limited. It is important to explore its biological effects and associated bioactive compounds, aiming to propose natural alternatives for pharmaceuticals and sustainable agriculture. Thus, this study aims to assess the bioactive properties of its leaves (RmL) through various extracts, including aqueous and hydroalcohol (1:1), obtained by means of ohmic heating extraction for 5 and 10 min (A5, A10, H5, H10). The extracts were evaluated for their antioxidant, antiproliferative, antibacterial, and insecticidal activities. Aqueous extraction demonstrated higher recovery of phenolic compounds such as gallic acid and catechin, while other compounds were also detected in lower concentrations (epicatechin gallate, ferulic acid, 2-hydroxycinnamic acid, and myricetin). All extracts showed antiproliferative activity against the A549 cell line (lung cancer), with less effect on the HeLa cell line (human cervix carcinoma), while none exhibited cytotoxicity against the noncancerous ARPE-19 cell line. Aqueous extracts displayed notable antimicrobial effects, particularly A10 against Staphylococcus aureus. In insecticidal assessments, H5 emerged as the most effective treatment against Musa domestica and Plutella xylostella. This study pioneers the evaluation of RmL extracts, revealing promising bioactivity with selective extraction conditions for further applications in various industrial fields.

Research of the Protein Profile and Allergenic Properties of the Tropomyosin and Other Allergenic Components in the Composition of Water-Salt Extract of Giant Tiger Shrimp (<i>Penaeus monodon</i>)

Despite the success in identifying new crustacean allergens other than tropomyosin, many potential allergens remain unidentified. At present there are no diagnostic and treatment crustaceans allergens on the Russian market, including tropomyosin of invertebrates. The aim of the research was to explore allergenic properties of tropomyosin and other proteins in water-salt extract from tiger shrimp (Penaeus monodon). Raw and boiled meat of giant tiger shrimp was used to prepare allergenic extracts. To identify the specific activity of experimental allergens, sera from patients allergic to crustaceans with an established degree of activity (class 3) were used. The levels of specific IgE were from 3.5 to 17.5 IU/mL. ELISA was performed with the allergen samples. Polyacrylamide gel electrophoresis of raw and boiled shrimp allergen preparations was followed by Western blotting with the most allergen-specific serum. It has been shown that the extracts from raw and boiled shrimp have allergenic activity (bind IgE). The heat treatment of shrimp had no effect on allergenic activity except for one sample, where a strong reaction with the antigens was found. It is proved that the selected extraction conditions make it possible to reveal the multifractional nature of the protein profile of raw and boiled shrimp extracts. In Western blotting experiments the raw shrimp extract showed a weak reaction; tropomyosin was not detected. At the same time five protein fractions were identified in the boiled shrimp samples which reacted with IgE antibodies of a patient with crustaceans’ allergy. The data obtained will allow us expanding the knowledge about crustacean allergy and continueing our research to determine the optimal conditions for cleaning shrimp allergens.

Effects of protease-assisted aqueous extraction on almond protein profile, digestibility, and antigenicity

Almonds (Prunus dulcis) are one of the most consumed tree nuts worldwide and have been recognized as a healthy and nutritious food. Nevertheless, almonds are also a source of allergenic proteins that can trigger several mild to life-threatening allergic reactions. The effects of selected extraction conditions (aqueous vs. protease-assisted aqueous extraction) on the protein profile determined by proteomics analysis of excised SDS-PAGE gel bands, in vitro protein digestibility, and immunoreactivity of almond protein extracts, were evaluated. Proteolysis altered almond protein sequential and conformational characteristics thus affecting digestibility and antigenicity. Proteomics analysis revealed that enzymatic extraction resulted in the reduction of allergen proteins and epitopes. While complete hydrolysis of Prunin 1 and 2 α-chain was observed, Prunin 1 and 2 β-chains were more resistant to hydrolysis. Protein in vitro digestibility increased from 79.1 to 88.5% after proteolysis, as determined by a static digestion model. The degree of hydrolysis (DH) and peptide content of enzymatically extracted proteins during gastric and duodenal digestion were significantly higher than the ones from unhydrolyzed proteins. Proteolysis resulted in a 75% reduction in almond protein immunoreactivity as determined by a sandwich enzyme-linked immunosorbent assay and a reduction in IgE and IgG reactivities using human sera. The present study shows that moderated hydrolysis (7% DH) using protease can be used as a strategy to improve almond protein digestibility and reduce antigenicity. This study's findings could further enhance the potential use of almond protein hydrolysates in the formulation of hypoallergenic food products with improved nutritional quality and safety.

Extraction of Rhenium and Osmium from Lead Technogenic Raw Materials of Copper Production.

Lead sludge from copper production is a source of rare metals, such as rhenium and osmium, whose content reaches 0.06–0.08% and 0.0025–0.0050%, respectively. The base of the sludge consists of lead sulfate. A method of reductive smelting of lead sludge from copper smelting production at 1000–1100 °C has been developed. Coke was used as a reducing agent and sodium sulfate as a slag-forming material. Optimal conditions for selective extraction of rare metals in smelting products were found: osmium in the form of metallic form into raw lead and rhenium in the form of perrhenate compound Na5ReO6 into sodium-sulfate slag. The developed technology makes it possible to extract rhenium with a high degree of extraction in the form of water-soluble compounds for the subsequent production of commercial salts of rhenium by the known hydrometallurgical methods. The content of rhenium in the slag phase is 0.18–0.25%, with its initial content in the slime of 0.06–0.08%. The degree of rhenium concentration at the first stage of processing is 3–3.2 times in the form of water-soluble perrhenate. Osmium and lead do not form solid solutions; osmium in crude lead is mainly concentrated in the lower zones of lead. A method of obtaining a concentrate containing 53–67% osmium from raw lead with an initial content of 0.0025–0.0050% in the slurry and a concentration number of 13,000–21,000 times has been proposed.

Combined Effect of Extraction and Purification Conditions on Yield, Composition and Functional and Structural Properties of Lupin Proteins.

Lupin meal presents great potential as an alternative plant-based source of proteins for human nutrition. In the present work, different conditions of extraction and purification were evaluated for production of lupin protein isolates. The results showed that the protein extraction yield was comparable at acidic and conventionally used alkaline extraction pH (37% vs. 40–45%, respectively). Proteins extracted were principally composed of globulins. The ionic strength negatively impacted the protein extractability at pH 2, whereas no significant differences were observed between extractions at 20 to 50 °C. The selected extraction conditions (pH 2 and 7) combined with purification by isoelectric precipitation or ultrafiltration process generated the isolate-grade products. Interestingly, further characterization revealed a partial denaturation of proteins extracted at pH 2 resulting in loss of protein solubility at pH 6 and 7 (10–50%), modifications in secondary structure, lower thermal stability, and formation of protein aggregates. However, foaming and emulsifying properties were generally similar for almost all lupin isolates. Further investigation might be of interest with regard to the extraction behaviours and structural and functional properties of specific lupin protein fractions.

Selective extraction performance of Ni, Cu, Co, and Mn adopted by a coupled leaching of low-grade Ni-sulfide ore and polymetallic Mn-oxide ore in sulphuric acid solutions

The coupled leaching of ocean polymetallic nodule and low-grade nickel sulphide ore in sulphuric acid solution was investigated, especially in performance on selective extraction of Ni, Cu, Co, and Mn. This work can be divided into three parts. First, the advantageous selective metal extraction conditions, parallel to the optimal coupled leaching conditions, were measured by coupled leaching tests which adopted the Ni, Mn, Cu, Co, and Fe dissolution efficiency. Under the optimal conditions, the extraction ratios of Ni, Mn, Cu, Co, and Fe are 96.8%, 97.3%, 92.2%, 97.9%, and 28.9%, respectively. Second, electrochemical tests revealed that multi-metal simultaneous extraction from two ores depends on the reduction-oxidation dissolution of a corrosion cell of the nodule cathode and the sulphide ore anode. The results showed that acidity and Fe3+ ion affected dissolution of both ores significantly; high valence manganese oxide reduction takes precedence which is in control of the Ni, Mn, Cu, and Co dissolution of the nodule; Ni, Cu, and Co extraction from the nickel ore is a course of sulphide minerals oxidative conversion which significantly affected by Fe2+-containing sulphide oxidation. Third, the separation performance of iron substance in the solution was determined by the transformation of minerals phases of the leached residues, showing that Fe-bearing minerals dissolved to Fe3+ ion then precipitated as iron vitriol or oxide during the selectively coupled leaching. The selectively coupled leaching of low-grade multi-metallic sulphide ore and oxide ore mainly rests with the transformation of Fe-containing species in the system.

Multiobjective decision making strategy for selective albumin extraction from a rapeseed cold-pressed meal based on Rough Set approach

This article proposes the application of multiobjective decision making strategy for selective albumin extraction by Pareto’s domain determination and ranking by Decision Engineering tool based on the Rough Set approach. In this study, both competing process performance indicators of rapeseed albumin extraction and quality of the solid residue remaining from this process were considered for an overall valorization of the rapeseed cold-pressed meal. The impact of extraction pH and NaCl concentration on three process performance indicators including the albumin extraction yield, the albumin content in the extract, and the phytic acid content in the remaining solid residue was studied. The results of the optimization approach showed that the high selectivity of rapeseed albumin extraction was to the detriment of the productivity of the process and the quality of the solid residue. The optimal conditions for selective rapeseed albumin extraction while producing a high-quality solid residue were identified at pH 2.0 and 0.11molL−1 of NaCl concentration. Upon these conditions, good albumin extraction yield was achieved (55.5%) with a high selectivity (97.9% of albumins in the extract). The isolate obtained after purification exhibited suitable color, high solubility, promising emulsifying properties and good foaming properties, which is of interest for food applications. Besides, the identifying extraction conditions yielded a protein-rich solid residue (35.6% on dry matter basis) with reduced phytic acid content (3.6% on dry matter basis), which can be used for feed applications.

Application of response surface methodology for modeling and optimization of the extraction and separation of Se(IV) and Te(IV) from nitric acid solution by Cyanex 301 extractant

The objective of this study is to develop a mathematical model based on the response surface methodology (RSM) for Liquid-liquid extraction and separation of Selenium and Tellurium from the aqueous nitric acid solution using Cyanex 301 as a potential organic extractant. For this purpose, three independent variables, i.e. nitric acid concentration (1–5 mol L−1), Cyanex 301 concentration (0.02–0.1 mol L−1), and extraction temperature (15–55 °C) were considered to evaluate their impacts on the responses of the percentage extractions (%E) of selenium and tellurium based on central composite design (CCD) approach. After conducting the experiments and statistically analyzing the results, correlations were proposed for selenium and tellurium extraction based on quadratic models. The results indicated that the Cyanex 301 concentration was the most paramount variable in extraction separation of Selenium and Tellurium. According to the obtained results the optimal condition for selective extraction of Se(IV) over Te(IV) was obtained at HNO3 concentration 2.7 mol L−1, Cyanex 301 concentration 0.06 mol L−1, and extraction temperature 25 °C. The optimum predicted extraction percentage of Se(IV) and Te(IV) was 99.77% and 28.47%, respectively and the actual values were 99.72%, and 28.12%, respectively. Also, the predicted and real separation factor was found to be 1089.87 and 910.37 respectively. These results showed the suitability of the implemented model and the prosperous application of RSM based on CCD in optimizing the selective extraction conditions of Se(IV) from Te(IV) in nitric acid medium.

Mexican Oregano (Lippia graveolens Kunth) as Source of Bioactive Compounds: A Review.

Lippia graveolens is a traditional crop and a rich source of bioactive compounds with various properties (e.g., antioxidant, anti-inflammatory, antifungal, UV defense, anti-glycemic, and cytotoxicity) that is primarily cultivated for essential oil recovery. The isolated bioactive compounds could be useful as additives in the functional food, nutraceuticals, cosmetics, and pharmaceutical industries. Carvacrol, thymol, β-caryophyllene, and p-cymene are terpene compounds contained in oregano essential oil (OEO); flavonoids such as quercetin O-hexoside, pinocembrin, and galangin are flavonoids found in oregano extracts. Furthermore, thermoresistant compounds that remain in the plant matrix following a thermal process can be priced in terms of the circular economy. By using better and more selective extraction conditions, the bioactive compounds present in Mexican oregano can be studied as potential inhibitors of COVID-19. Also, research on extraction technologies should continue to ensure a higher quality of bioactive compounds while preventing an undesired chemical shift (e.g., hydrolysis). The oregano fractions can be used in the food, health, and agricultural industries.

Selective extraction of napins: Process optimization and impact on structural and functional properties

There is a growing worldwide demand for alternative sources of proteins for human nutrition. In this context, many researches have been carried out to develop an original process for production of total proteins from rapeseed meal. Interestingly, some recent works have demonstrated a possible selective extraction of napins (rapeseed albumins). However, the precise impact of extraction conditions on process performances has never been elucidated. The aim of this study was to establish the optimal conditions for selective extraction of napins from rapeseed meal while producing a high-quality solid residue. First, the effect of pH (2–4) and NaCl concentration (0–0.2 mol.L−1) at 20 and 55 °C on the extraction process performances was investigated by design of experiments. Second, a rational approach of multicriteria optimization including genetico-evolutionary algorithm was employed. As a result, two sets of optimal conditions (pH 2.0/0.11 mol.L−1 of NaCl at 20 °C and pH 3.75/0.2 mol.L−1 of NaCl at 55 °C) were found. They allowed for >55% of napin extraction yield, >95% of napin proportion in the extract and <4% of phytic acid content in the solid residue. However, much greater yield of napins was noted at the higher extraction temperature (55.4% vs 75.56% at 20 and 55 °C, respectively). Napins extracted under the two optimal conditions and purified by ultrafiltration had a light creamy color and similar composition. Minor structural modifications between the two proteins were observed, but they did not affect the functional properties (foaming and emulsifying properties) that appeared to be comparable.

Supercritical Fluid Chromatography development of a predictive analytical tool to selectively extract bioactive compounds by supercritical fluid extraction and pressurised liquid extraction

Selective extraction is a great concern in the field of natural products. The interest is to apply specific conditions favouring the solubility of targeted secondary metabolites and avoiding the simultaneous extraction of unwanted ones. Different ways exist to reach selective extractions with suited conditions. These conditions can be determined from experimental studies through experimental design, but a full experimental design takes time, energy, and uses plant samples. Prediction from varied solubility models can also be applied allowing a better understanding of the final selected conditions and eventually less experiments.The aim of this work was to develop and use a chromatographic model to determine optimal extraction conditions without the need for numerous extraction experiments. This model would be applied on the selective extraction of the desired antioxidant compounds in rosemary leaves (rosmarinic and carnosic acids) vs chlorophyll pigments to limit the green colour in extracts. This model was achieved with Supercritical Fluid Chromatography (SFC) and then applied to Supercritical Fluid Extraction (SFE) and Pressurised Liquid Extraction (PLE) assays.SFC models predicted low solubility of chlorophylls for low (5%) and high (100%) percentage of solvent in carbon dioxide. Also, low solubility was predicted with acetonitrile solvent compared to methanol or ethanol. This was confirmed with different extractions performed using SFE with different percentages of solvent (5, 30, and 70%) and with the three solvents used in the SFC models (acetonitrile, methanol and ethanol). Also extractions using PLE were carried out using the same neat solvents in order to confirm the SFC models obtained for 100% of solvent. Globally, extractions validated the SFC models. Only some differences were observed between ethanol and methanol showing the complexity of plant extraction due to matrix effect. For all these extracts, the content of carnosic acid and rosmarinic acid was also monitored and selective extraction conditions of bioactive compounds could be determined.

High effective extraction of selected anthraquinones from Polygonum multiflorum using ionic liquids with ultrasonic assistance

In recent years, the toxicity of Polygonum multiflorum has been attributed to the anthraquinones. Therefore, the selective removal of anthraquinones will effectively improve the safety of Polygonum multiflorum. An ionic liquid-based extraction was firstly proposed to selectively extract anthraquinones from herbal powders with ultrasonic assistance. The relationship between selective extraction effect and important extraction conditions was investigated. Furthermore, the mechanism of the selective extraction was explored with the extraction kinetics and computation method. In addition, the recovery of ionic liquids was also investigated. Finally, high extraction efficiency (97.2%) and good selectivity (7.32) for anthraquinones from Polygonum multiflorum were achieved, and the ionic liquid was recovered with satisfactory recovery rate. It could provide a promising alternative method to isolate anthraquinones from other natural products.

Water Ultrasound-Assisted Extraction of Polyphenol Compounds from Brewer's Spent Grain: Kinetic Study, Extract Characterization, and Concentration.

Brewer’s spent grain (BSG) was chemically characterized obtaining 52.1% of carbohydrates, 17.8% protein, 5.9% lipids, 13.5% insoluble lignin and 24.3% of water-soluble extractives. This work has been focused on the study of polyphenol extraction of the extractive fraction by water ultrasound-assisted extraction. Selected extraction conditions were 47 °C and 21.7 mL water/gdry-BSG. The effect of solvent polarity on polyphenol extraction was studied by using ethanol aqueous mixtures, from 20% to 100% ethanol. The kinetics of polyphenol extraction have been fitted to the power law and the Weibull models yielding mean values of the root mean square deviation lower than 7.5%. Extracts have been characterized in terms of quantification of individual phenolic compounds by HPLC-DAD and protein and sugar soluble fractions (glucose, xylose, and arabinose). Polyphenol profile has been compared with other hydrolytic techniques, such as acid, basic and enzymatic hydrolysis, showing that ultrasound was not as effective as basic hydrolysis to release the phenolic acids esterified to the cell wall. A further centrifuge ultrafiltration concentration step was able to yield a retentate enriched in the protein fraction while individual phenolic compounds where mainly transferred to the permeate.

Protein extraction and sludge dewatering performance of ultrasound-assisted enzymatic hydrolysis of excess sludge.

Excess sludge contains a high amount of protein, which can be recovered to prepare protein foaming agents and other products with high added value. Enzymatic hydrolysis (EH) is a promising technology for the recovery of protein from excess sludge, and ultrasound has been identified as a potential method to assist in sludge disintegration. Ultrasonic pretreatment was combined with alkaline protease hydrolysis to extract protein from excess sludge produced by A2/O treatment (S1) and an oxidation ditch treatment (S2), and the extraction effects and changes in sludge dewatering performance were studied. The effects of the six factors ultrasonic power density, ultrasonication time, enzyme dose, pH, hydrolysis temperature and hydrolysis time were analyzed. The results showed that the ultrasound-enhanced enzymatic method could effectively extract sludge protein. Although the extraction efficiencies for the different municipal sludges were different, their extraction conditions were relatively similar. Considering the protein extraction rate and sludge dewatering performance, the selected extraction conditions were as follows: ultrasonic power density, 1W/mL; ultrasonication time, 20min; enzyme dose, 3500U/g; pH11; hydrolysis temperature, 60°C; and hydrolysis time, 3h. Under these conditions, the protein extraction rate (Rp) of S1 and S2 reached 55.9% and 52.3%, respectively. Moreover, the improvement in sludge dewatering performance (Dw) of S1 and S2 was 49.5% and 52.4%, respectively. Comparison of the protein, polypeptide, and amino acid contents obtained from ultrasound-assisted enzymatic hydrolysis (UEH), EH, and ultrasonic hydrolysis (UH) further demonstrated the beneficial effect of ultrasound application on enzymatic hydrolysis.

Protic Ionic Liquids as Efficient Solvents in Microwave-Assisted Extraction of Rhein and Emodin from Rheum palmatum L.

Rheum palmatum L. (R. palmatum L.) is a traditional Chinese herb and food, in which rhein and emodin are the main bioactive components. The extraction of the two compounds from R. palmatum L. is, thus, of great importance. In this work, protic ionic liquids (PILs) were applied in the microwave-assisted extraction (MAE) of rhein and emodin from R. palmatum L., which avoids the toxicity of organic solvents. The results of the present study indicate that PILs possessing higher polarity exhibit higher extraction ability due to their stronger absorption ability for microwave irradiation. Compared with conventional solvents, such as methanol, trichloromethane, and deep eutectic solvents (DESs), the PIL, 1-butyl-3-himidazolium methanesulfonate ([BHim]MeSO3) reported herein is more efficient. The selected extraction conditions of liquid–solid ratio, microwave irradiation time, microwave irradiation power, and PIL concentration were 40 g·g−1, 50 s, 280 W, and 80%, respectively. Under the selected conditions, the extraction yields of rhein and emodin were 7.8 and 4.0 mg·g−1, respectively. These results suggest that PILs are efficient extraction solvents for the separation of active components from natural products.

Microwave-assisted extraction of antioxidant compounds from sunflower hulls

The objective was to determine the adequate conditions for the microwave-assisted extraction of antioxidant compounds from the seed hull of sunflower hybrids. The existence of genetic and environmental variability in the phenolic content obtained under the selected extraction conditions was also analyzed. The extractions were carried out at 70 °C-20 and 90 °C-10 min, using water as solvent and a power of 600 W. The total phenol, flavonoid and antioxidant activity were evaluated. The microwave extraction process at 90 °C-10 min gave significantly higher values of total phenol (407.13 ± 6.11–512.71 ± 23.54 mg gallic acid⋅100 g−1 hull), flavonoids (210.09 ± 6.15–297.64 ± 5.68 mg catechin⋅100 g−1 hull) and antioxidant activity (76.73 ± 4.40–110.80 ± 3.51 μmol TE⋅g−1 hull) than those obtained at 70 °C-20 min. The cultivation environment also significantly affected the antioxidant yield, with total phenol and flavonoid contents being significantly higher for the hybrids grown in Balcarce than for those from Tandil. A significant interaction between hybrids and cultivation environmental was also observed for the antioxidant activity, indicating that the environmental effects were not similar among hybrids. The results of this study provide valuable information related to giving added value to a residue of the oil industry.

English

Shea butter is a high–value shea nut fat used as an edible oil, antimicrobial and moisturiser in the food, pharmaceutical and cosmetic industries, respectively. The annual worldwide export of shea nut from Africa is 350,000 MT of kernels with a market value of approximately $120 million to producing countries. The multifunctional properties of the shea butter depend strictly on its compositional properties: the peroxide value, moisture content, free fatty acid level and the insoluble impurities. Standard extraction technologies: the traditional, mechanized, enzymatic and chemical methods were used for shea butter extraction. Current extraction technologies which rely on different extraction parameters for shea butter extraction are yet to yield the desired qualities and efficiencies of butter. Application of hydrolysing enzymes during enzyme extraction however eliminates the laborious, tedious and labour–intensive extraction processes creating alternative, selective and mild extraction conditions. The current review gives an overview of shea butter extraction technologies, the efficiencies, qualities and a perspective into the shea butter industry. Key words: Shea butter, mechanical, chemical, traditional, enzymatic, technologies.

Using Extractables Data of Sterile Filter Components for Scaling Calculations.

Users of single-use (SU) components need extractables data to demonstrate material safety for regulatory bodies before incorporation in the biopharmaceutical process. In this context, the correct use of such extractables data is key to deriving realistic risk assessments for SU devices. In this paper, a standardized extractables approach was used that provides comprehensive extractables information including identity and quantity. The combination of extractables data obtained from different components of a sterile filter capsule, such as the filter cartridge and housing, and the scaling thereof is presented. A sterile filter type including polyethersulfone membrane was extracted with pure water and pure ethanol at 40°C for 24 h. The organic extractables were identified and their concentration quantified using state-of-the-art analytical methods such as gas chromatography-mass spectrometry for semivolatile compounds together with headspace sampling for volatile compounds, and liquid chromatography coupled with high-resolution mass spectrometry. The extractables detected were assigned to the materials of filter construction. The evaluation showed that the extractables quantities per device depended on the surface areas of the contact materials, such as the filter membrane, and also on the plastic parts. This paper confirms the validity of a so-called component approach and a scaling concept to calculate extractables data for SU filters of different sizes with short-term contact.LAY ABSTRACT: In the biopharmaceutical industry, a large number of SU system combinations with a variety of different sizes are used. Suppliers of such diverse SU systems and assemblies cannot perform extraction studies for all of the different configurations and sizes individually. It is acceptable in this industry to use component approaches and scaling concepts to provide extractables data for SU systems and assemblies derived from a dedicated extraction experiment. This paper shows the applicability of a so-called component approach and of a scaling concept to calculate extractables data for sterile polyethersulfone membrane filters and filter capsules of different sizes. Selected extraction conditions allow scaling calculations according to underlying physical principles. The extractions were performed under short-term contact, for example, 24 h, to ensure that the release of extractables was diffusion-controlled. The results demonstrated that extractables quantities depend on the surface area of the contact material. Membrane-related compounds were scalable with the membrane area, whereas polypropylene (PP)-related compounds were scalable with the PP contact area.

Hydrometallurgical recovery of Zn(II) and Mn(II) from alkaline batteries waste employing aqueous two-phase system

Abstract In this study, a greener method for the recovery of zinc and manganese from alkaline batteries waste was developed using Aqueous Two-Phase System (ATPS). ATPS is a liquid-liquid extraction technique. Zn(II) and Mn(II) were extracted using the diluted liquor from samples of spent alkaline batteries, and the experimental conditions were evaluated considering the effects of the following parameters: (i) nature and concentration of the extractants (1-(2-pyridyl-azo)-2-naphthol (PAN), (bis-4-trimethylpentyl) phosphinic acid (Cyanex 272), diphenylthiocarbazone (dithizone, C13H12N4S) and bis-(2-ethylhexyl) phosphoric acid (D2EHPA)); (ii) pH (3.00, 6.00 and 11.0), (iii) ATPS-forming electrolytes (Na2SO4, C6H5Na3O7 or C4H4Na2O6); (iv) ATPS-forming polymers (L35 and L64); and (v) tie-line length (TLL) and mass ratio between top and bottom phases (mTP/mBP). The recovery efficiency was evaluated using the extraction percentage (%E) and separation factor ( S Zn / M n ) between Zn(II) and Mn(II). The best conditions for selective extraction of the metal ions were achieved using an ATPS composed by L64 + Na2SO4 + H2O at pH = 3.00, TLL = 41.83% w/w and mTP/mBP = 1 using dithizone as the extracting agent and leach liquor with dilution factor equal to 10. This resulted in a value for separation factor of S Zn / M n = 1.2 × 106, in one extraction stage.