Anion Column Research Articles

Recovery of carboxylic acids from actual effluent by using sequential cationic-anionic adsorption steps at semi pilot scale

This work presents for the first time an exhaustive experimental assessment at semi-pilot scale for the sequential use of cationic-anionic adsorption columns for recovering carboxylic acids (CAs) from a real fermentation broth. The consecutive steps were dedicated to i) remove cations limiting the CAs interaction with the functional group of the anionic resin, and ii) adsorb CAs onto the anionic resin, respectively. The experimental broth was obtained from anaerobic co-fermentation of urban biowaste (UBW-broth). Breakthrough (BT) tests were firstly performed with the cationic column containing the strong-acid resin Lewatit® S2568H. This allowed both to assess the single process and to prepare 60 L of decationised UBW-broth to be used in the BT-tests with the anionic column (containing the weak-basic resin Lewatit® A365). Both columns were assessed (at 25°C) under packed and expanded bed modes, by feeding at different rates the actual UBW-broth or synthetic solutions. Main study innovative outputs were: 1) 100 % of the CAs occurring in UBW-broth were recovered with the proposed system; 2) best performances were obtained under expanded bed mode of operation, allowing to use 100 % of the installed capacity; 3) the affinity of other organic matter else than CAs resulted weaker than Na+/NH4+ and CAs/PO4x-/Cl- in both cationic and anionic columns, respectively (i.e. low adsorption performances generally reported are due to inorganic cations/anions presence); 4) a very preliminary economic analysis carried out on the basis of the obtained data indicates overall costs ranging 0.58–1.49 EUR/kg of CAs (depending on the process configuration).

Atomic imaging and optical properties of InAs/In0.5Ga0.5As0.5Sb0.5 type II superlattice

High-quality III–V quantum structures, advanced epitaxial technologies, and characterization methods are essential to drive the development of infrared optoelectronic materials and devices. As an important component of type II superlattices, InAs/InxGa1−xAsySb1−y would play an important role in the field of high-performance infrared detectors due to their excellent luminescence efficiency and high crystal quality. However, their interfacial characteristics and the associated minority carrier lifetime are still difficult to identify. In this paper, an atomic imaging technique was used to identify the arrangement and distribution of elements of the InAs/In0.5Ga0.5As0.5Sb0.5 superlattice. Our results confirm the epitaxy mechanism that the quaternary alloy consists of two kinds of ternary alloy in one monolayer. Moreover, by separating the cation and anion columns in the elementally resolved atomic images of the InAs/In0.5Ga0.5As0.5Sb0.5 superlattice, we demonstrate that the interfacial atomic intermixing is less than one molecular layer thickness. Therefore, benefiting from excellent interface quality, InAs/In0.5Ga0.5As0.5Sb0.5 superlattice exhibited high radiation recombination efficiency in the long-wave infrared band (∼8.5 μm), and longer minority carrier lifetime (∼810 ns at 90 K).

The OH stretching region in infrared spectra of the apatite OH-Cl binary system

Abstract Polarized Fourier Transform Infrared (FTIR) microspectroscopy of the OH stretching region of hydroxylapatite-chlorapatite solid solutions presents novel problems for the assignment of peaks to specific OH-Cl pairs. Crystal structure refinements of Hughes et al. (2016) identified new positions for column anions in synthetic mixed Cl-OH apatites, with three different column anion arrangements depending on composition. These structural refinements, combined with bond valence calculations, allow for interpretation of the OH stretching region. A peak at 3574 cm-1 is identified as that from end member hydroxylapatite. A second major peak at 3548 cm-1 is only found in mixed chlorapatite-hydroxylapatite solid solutions, as is a third peak at 3592 cm-1. Both represent perturbations of the OH stretching vibration as compared to hydroxylapatite, to lower and higher frequency, respectively. Both of the new peaks are the result of a Clb-OH sequence, with adjacent anions in crystallographically similar positions, both above or both below adjacent mirror planes. One configuration has the hydrogen atom pointed towards the chlorine atom. The second has the hydrogen of the OH group pointed away from the chlorine atom. Both configurations present novel problems. The shift to lower wavenumber at 3548 cm-1 is characteristic of hydrogen bonding in fluorapatite-hydroxylapatite mixtures, yet the distance between O(H) and Clb is too great to allow it. The shift of OH stretching vibrations to lower wavenumber is produced through changes in polarization of intervening Cl-Ca2’ (or Ca2) and Ca2(’)-O3 bonds, which are affected by the presence of the large chlorine atom. Lowering the OH stretching vibration mimics the expected effect of a chlorine on a neighboring OH group in the apatite c-axis column, though without hydrogen bonding. The shift to higher wavenumbers, i.e. higher frequency at 3592 cm-1, is the opposite of that expected for hydrogen bonding between column anions in the apatite mineral group. It is ascribed to interaction between an adjacent Clb and the oxygen end of an adjacent OH dipole. This pairing places an oxygen and a chlorine atom in close proximity. Possible means of accommodation are discussed. A ubiquitous peak at 3498 cm-1 represents hydrogen bonding between an OH and the OHa site, with an interoxygen distance of about 2.9 Å. Published modeling supports the hypothesis that the OHa site is occupied by an O rather than an OH. However, no clear counterpart to this pairing is observed in crystal structure refinements for specimens lacking OHa, although the infrared absorbance is present. The existence of oxyapatite is inferred from studies of plasma-sprayed biomaterials, but the crystallographic details of the substitution have remained elusive. A minor shoulder at 3517 cm-1 does not have a clear counterpart in the structural refinements. Sequences of three columnar anions (e.g. OH-Cl-OH or Cl-OH-OH) can be ruled out, but unequivocal assignment awaits further research.

Research Progress of Bioactive Components in Sanghuangporus spp.

The species in Sanghuangporus are a group of edible mushrooms with a long history of oral use in East Asia as a health-improvement method. They should be classified under the genus Sanghuangporus rather than mistakenly in Phellinus or Inonotus. The major components in this genus consist of polysaccharides, polyphenols, triterpenoids, and flavonoids, all of which exist in the fruiting bodies and mycelia. For extraction, studies have shown methods using hot water, ethanol, DES solvent, and alkaline, followed by purification methods including traditional anion column, Sevag solution, macroporous resin, and magnetic polymers. Proven by modern medical technology, these components possess promising anti-inflammatory, antioxidative, antitumor, and immunoregulation effects; additionally, they have health-improving effects including pulmonary protection, hypoglycemic properties, sleep improvement, gout mitigation, antiaging, neuroprotection, and muscle-strengthening abilities. Several toxicity studies have revealed their safety and recommend a dose of 1 g/kg for mice. As a newly emerged concept, functional food can provide not only life-sustaining nutrients but also some health-improving effects. In conclusion, we substantiate Sanghuang as a functional food by comprehensively presenting information on extraction and purification methods, component medical and structural properties, and nontoxicity, hoping to benefit the development of Sanghuang species as a group of functional food.

Determination of Human Epidermal Growth Factor in Cosmetics by Solid Phase Extraction (SPE) with High-performance Liquid Chromatography – Tandem Mass Spectrometry (HPLC-MS/MS)

A method for determining human epidermal growth factor (hEGF) in cosmetics was developed using solid-phase extraction with high-performance liquid chromatography – tandem mass spectrometry. The sample was extracted and purified by a mixed anionic solid-phase extraction column (MAX), and the eluent was passed through a nylon filter membrane into a polypropylene vial. The matrix-matched external standard method was used to quantify the analyte in multi-reaction monitoring mode. The analyte had an excellent peak shape within 11 min with a linear range from 5 to 80 ng/mL and a linear correlation coefficient (r) of 0.9995. The limit of detection and limit of quantification were 0.75 and 2.5 μg/kg, respectively. The recovery of the target was from 81.5% to 88.8%, and the relative standard deviation was between 1.16% and 5.07%. The results met the International Organization for Standardization 12787 standard. The established method was successfully applied to 30 cosmetic samples. The proposed method is sensitive, accurate, reliable, and suitable for the quantitative confirmation of hEGF and monitoring its illegal addition to cosmetics.

Development and inter-laboratory validation of analytical methods for glufosinate and its two metabolites in foods of plant origin.

Glufosinate is widely used to control various weeds. Glufosinate and its main metabolites have become the focus of attention because of their high water solubility and persistence in aquatic systems. Quantification of the agrochemical product and its metabolite residues is essential for the safety of agricultural products. In this study, a highly specific, simple method was developed to directly determine glufosinate and its metabolite residues in 21 plant origin foods by liquid chromatography with tandem mass spectrometry (LC-MS/MS), and it was validated on 11 foods in five laboratories. Finally, the repeatability limit, reproducibility limit, and uncertainty of the method were calculated based on these validated data and used to support the more accurate detection results. Four different chromatographic columns were used to analyze three target compounds, and the anionic polar pesticide column showed the optimum separation and peak shape. Composition of the mobile phase, extraction solvent, and the clean-up procedure were optimized. The developed method was validated on 21 plant origin foods. The average recoveries were 74-115% for all matrices. The validation results of five laboratories showed this method had a good repeatability (RSDr < 9.5%) and reproducibility (RSDR < 18.9%). The method validation parameters met the requirements of guidance established by the European Union (EU) and China for pesticide residue analysis. This methodology can be used for a routine monitoring that performs well forglufosinate and its metabolite residues.

An analytical method for the determination of glyphosate and aminomethylphosphoric acid using an anionic polar pesticide column and the application in urine and serum from glyphosate poisoning patients.

An analytical method for the determination of glyphosate (GLY) and aminomethylphosphoric acid (AMPA) in biological fluid samples (serum and urine) from poisoning patients using liquid chromatography-tandem mass spectrometry (LC-MS/MS) is established. After the sample pretreatment, including protein precipitation and a modified liquid-liquid extraction method, the chromatographic separation was conducted on a trifunctional modified hydrophilic column. The mobile phases in the gradient program were 2.5% formic acid aqueous solution and acetonitrile. The multiple reaction monitoring (MRM) models and the isotope-labeled internal standards were used in the acquisition process. Good linearities and satisfying recovery rates were obtained in two sample matrices with good RSDs. The detection limits of GLY and AMPA were <2 μg L-1, which were close to those obtained in our previous research. The established method was applied to biological samples from five patients with glyphosate intoxication. The analysis of the trend for the concentration of GLY and AMPA in two biological samples was investigated, and the difference in the downward trend of AMPA in urine was found in patients with a relatively higher concentration of GLY in serum.

Arylene Diimide Derivatives as Anolyte Materials with Two-Electron Storage for Ultrastable Neutral Aqueous Organic Redox Flow Batteries

Arylene Diimide Derivatives as Anolyte Materials with Two-Electron Storage for Ultrastable Neutral Aqueous Organic Redox Flow Batteries

Determination of Glyphosate in White and Brown Rice with HPLC-ICP-MS/MS.

In 2017, the European Commission renewed the approval of glyphosate (GLY) but only for five years. GLY remains one of the most controversial and studied molecules. A simplified method was tested for the determination of GLY in white rice (WR) and brown rice (BR), after extraction only with a methanol solution, by liquid chromatography coupled with inductively coupled mass triple quadrupole (HPLC-ICP-MS/MS) with a PRP-X100 anionic column. After performing a test on groundwater, the quantification of GLY in WR and BR was validated in terms of the LOD, LOQ, accuracy, precision, linearity, and the matrix effect. The LOD was 0.0027 mg kg-1 for WR and 0.0136 mg kg-1 for BR. The LOQ was 0.0092 mg kg-1 for WR and 0.0456 mg kg-1 for BR. The mean recoveries were within 76-105% at three fortification levels. The relative standard deviation for the analysis (five replicates for three spike levels) was &lt; 11% for both matrices. A linear response was confirmed in all cases in the entire concentration range (R2WR = 1.000 and R2BR = 0.9818). The proposed method could be considered useful for the determination of GLY in different types of rice and designed and adapted for other cereals. The matrix effect, quantified in BR matrix extraction, could be avoided by using a matrix-matched calibration line.

Invertebrate fauna in municipal wells in Kraków, Poland

This study of fauna in municipal wells continues our previous investigations performed in rural areas (Dumnicka et al. 2017). The invertebrate fauna of city wells was rarely studied: by Vejdovský (1882) and Řehačkova (1953) in Prague, Jaworowski (1893) in Kraków and recently by Koch et al. (2020) in Karlsruhe. In 2019-2020 studies of fauna composition and water chemistry were done twice (spring-summer and autumn period) in 91 wells situated in various parts of the Kraków city. This work evaluated fauna distribution and diversity with patchy bedrock geological structure and local water pollution. Water temperature and conductivity were measured in situ using a portable Elmetron CX-742 pH meter. In contrast, chemical analyses were done in the laboratory with DIONEX ICS 2000 unit and a DIONEX ICS 5000 unit, equipped with a DIONEX AS18 anion column and a DIONEX CS16 cation column. For fauna studies, 100 l of water was filtered by a plankton net (50 μ m mesh size), and invertebrates were sorted in vivo under a stereoscopic microscope with 10x magnification. The material was determined to family level, except for Rotifera. Our results showed that water chemistry in Kraków wells varied strongly spatially and between sample collection times – this was also stated by various authors and summarized by Chowaniec et al. (2007). The depth of the wells varied from 5.0 to 100 m. Water temperature was relatively high (average value 12.95 ±1.4 o C) and pH almost neutral (7. 13 ±0.34). Water conductivity values were very high (1324.3±572 µS) due to high concentrations of calcium (170.3±66 mg L-1), sulfates (151.8±81.4 mg L-1), and less frequently chlorides (155.5±143.7 mg L-1). In many wells, ammonium ion was present (0.354±0.764 mg L-1), whereas, in other samples, nitrate concentrations varied strongly from 0.1 to 130.5 mg L-1 (average value 21.92±27 mg L-1). The occurrence of invertebrates (at least from one taxonomic group) was stated in 74 wells. Copepoda (family Cyclopidae) were found most frequently (in 40 wells) and in highest numbers (it means that in some wells several dozens of individuals were caught). Nematods and annelids were stated in 19 and 17 wells respectively, but in small number. The remaining groups, such as turbellarians (Catenulida and Rhabdocoela), rotifers and ostracods were present in a few wells only, while amphipods (Niphargus tatrensis morphospecies) exclusively in two wells. Moreover, dipterans larvae (from families: Anisopodidae, Chironomidae, Culicidae, Empididae, Limoniidae, Psychodidae and Rhagionidae) were found in 13 wells, whereas Collembola, considered to be terrestrial fauna, were found in 49 wells. In the majority of cases all springtails and fly larvae were alive. The presence of Diptera and Collembola inside the wells might result from leak of pump mechanisms therefore these invertebrates could just survive for some time inside pumps. The occurrence of invertebrates (at least from one taxonomic group) was started in 74 wells. Copepoda (family Cyclopidae) was found most frequently (in 40 wells) and in the highest numbers (it means that in some wells, several dozens of individuals were samples). Nematodes and annelids were stated in 19 and 17 wells, respectively, but in small numbers. The remaining groups, such as turbellarians (Catenulida and Rhabdocoela), rotifers, and ostracods, were present in a few wells, while amphipods (Niphargus tatrensis morphospecies) exclusively in two wells. Moreover, dipterans larvae (from families: Anisopodidae, Chironomidae, Culicidae, Empididae, Limoniidae, Psychodidae, and Rhagionidae) were found in 13 wells, whereas Collembola, considered to be terrestrial fauna, were found in 49 wells. In the majority of cases, all springtails and fly larvae were alive. The presence of Diptera and Collembola inside the wells might result from the leak of pump mechanisms; therefore, these invertebrates could just survive for some time inside pumps. Statistical analysis (Student t-test) revealed that the presence of fauna was not dependent on the depth of the wells (p ˂ 0.12). The effect of water pollution (expressed as increased concentrations of ammonium and chloride ions) on the presence of fauna was also not statistically significant, except for sulfide ions (p ˂ 0.058). In wells situated close to small running waters located on karstic bedrock or alluvial sediments, the presence of stygobionts (Niphargus tatrensis morphospecies, Trichodrilus cernosvitovi and Typhlocypris cf. eremita) was stated, whereas in wells situated along Vistula River no aquatic fauna was found probably due to the impermeable clay layer, which isolated wells water from water table of the river. The only study of fauna in dug municipal wells in Kraków made by Jaworowski (1893) showed higher water pollution than was found in this study: the crustaceans were found rarely, whereas ciliates were abundant and diversified. Collected material demonstrated the occurrence of relatively rich invertebrate fauna in subterranean city waters, but the effect of various parameters on its distribution has not been firmly established.

Application of radio-analytical technique for determination of “Age” of nuclear materials for nuclear forensics

Determination of “Age” – the time elapsed since the last chemical purification – of a nuclear material is an important parameter in Nuclear Forensic analysis. Estimation of age may give crucial acumen of the possible production facility and the declared origin – if available – in case of a suspected nuclear material which is out of regulatory control. Mass spectrometry is the most common analytical technique used for chronological studies due to its superior precision (lower uncertainty). Though alpha spectrometry can be used for age determination, it better suits for irradiated fuel based radio-chronology because of higher specific activity of irradiated actinides (actinides formed by irradiation of actinides within a reactor) like plutonium. This paper describes the application of alpha spectrometry for the age determination in some natural U-metal samples with known history. The method utilises the radioactive non-equilibrium existing between 234U and 230Th isotopes in the sample for the elucidation of age of the material. Optimisation of a chemical procedure for the separation of ultra-trace amount of thorium isotopes from bulk uranium material using double column anion exchange chromatography is also presented. The chemical recoveries of uranium and thorium obtained with the present method were >95%. The uncertainty in age determination was <10% and ∼15% for older (∼51 years) and newer (∼11 years) samples respectively. The method is also used to elucidate the age of an unknown uranium material and found to be 39 ± 4 years old.

Wild shrimp have an order of magnitude higher arsenic concentrations than farmed shrimp from Brazil illustrating the need for a regulation based on inorganic arsenic

BackgroundShrimp is a worldwide food commodity, it is a source of several nutrients and vitamins; however, this food is one of the major sources of arsenic for humans. Legislation around the world set limits for the concentration of this element in crustaceans but is mainly concerned with total analysis. Although, arsenic species have different toxicities and total analysis could be ineffective for making decisions about food security. MethodsSamples of wild (Farfantepenaeus brasiliensis) and farmed shrimps (Litopenaeus vannamei) from NE Brazil were fractionated in subsamples of carapace, muscle tissue and viscera. The whole shrimp as well as the animal tissue fractions were decomposed using microwave digestion and total arsenic was analyzed by mass spectrometry inductively coupled plasm (ICP-MS). The water-soluble arsenic species were extracted, and the extract was carried for speciation analysis using HPLC-ICP-MS with an anionic and cationic column. ResultsTotal As in wild shrimp samples exceeded Brazilian and USA food legislation by one order of magnitude, with concentrations of 11.5 ± 0.5 mg kg−1, while farmed shrimp had significantly lower total arsenic levels (0.53 ± 0.09 mg kg−1). More than 60% of the As was in the edible fraction in the wild shrimp, while in farmed shrimp this was less than 50%. The speciation analysis showed that arsenobetaine (AsB) was the predominant As form and iAs was below the Chinese legislation levels (iAs <0.50 mg kg−1) for shrimp in both species. ConclusionThe arsenic uptake in wild and farmed shrimp was discussed and some differences were found related to feed and salinity. About legislation, it has been concluded that most food legislations that consider only tAs are not appropriate to assess the toxicity of As in seafood. It is necessary to update the legislation of food control agencies to insert As speciation analysis in their protocols.

Biotransformation of urea in the water of water bodies

Introduction. The transformation of substances is an urgent problem of environmental hygiene. Urea (carbamide) is a product of human and animal life - enters water objects with household collector wastewater, surface runoff in areas that use urea as fertilizer, waste discharges from livestock complexes, and effluents of enterprises that produce carbamide. Two aspects of the problems associated with urea contamination of water bodies can be identified: the lack of a direct instrumental method for controlling urea and the lack of a comprehensive approach to controlling urea and its biotransformation products: ammonium, nitrites and nitrates. These two factors determined the relevance of the research. Materials and methods. The studies used the «Stayer» ionic chromatography system with anionic and cationic separation columns: Phenomenex Star-Ion A-300 100/4.6 USA; Shodex IC YS-50 150/4.6 Japan; when developing the urea analysis method, the «Aquilon» cationic column AQULINE C1P, 5µ,150/4.6 was used. The detection is conductometric and amperometric. The research objects were: surface, bottled, tap water, model water solutions of carbamide. As a urease source, the soil (sod-podzolic) from the Educational and Experimental Soil-Ecological Center of the Lomonosov Moscow State University “Chashnikovo” was used. Results. A new highly sensitive ion chromatographic method for determining urea in the water of various water bodies with a sensitivity of 5 mg/dm3 with direct sample input and using sample preparation - 0.5 mg/dm3 is proposed. The results of studies of model aqueous solutions of urea, surface water, tap water of Moscow, many bottled water samples on the content of urea and products of its biochemical transformation are presented. The presence of urea in the surface water and tap water of Moscow was revealed, and a correlation between the urea content and ammonium ions, nitrites and nitrates in the water was stated. Limitations of the study. The studies were carried out with waters whose total mineralization did not exceed 15 mg-eq/dm3 (water of river Don), and the urea content established in the water samples was not lower than 0.5 mg/dm3. Conclusion. When monitoring urea contamination of various water bodies, it is necessary to consider the products of its biotransformation under the action of urease, for as a result of the processes of urea biotransformation, a low-toxic substance can form more toxic products: nitrites, nitrates and ammonium. Applying the kinetic approach to study the processes of urea biotransformation in water under model conditions showed that the extreme type of kinetic curves corresponds to the formation of intermediate products - nitrites, and the increasing type corresponds to the formation and accumulation of final products - nitrates and ammonium ions.

Effective and rugged analysis of glyphosate, glufosinate, and metabolites in Tenebrio molitor larva (mealworms) using liquid chromatography tandem mass spectrometry

Tenebrio molitor larva (mealworms) has recently attracted attention as a protein source for food and feed. The larva is generally fed with wheat bran, which can be possibly contaminated with glyphosate. To establish food safe standards, a rugged and effective analytical method for glyphosate, aminomethylphosphonic acid, glufosinate, and their metabolites including 3-methylphosphinico-propionic acid, and N-acetyl glufosinate, in mealworms was optimized using liquid chromatography tandem mass spectrometry. An anionic polar pesticide column was used due to its high suitability for glyphosate. Acidified water and acetonitrile were used to extract the target compounds without contribution from various fatty and pigment interferences derived from brownish insects. Seven different clean-up procedures ((1) 50 mg C18 (2) 20 mg C18/Z-sep (3) PRiME hydrophilic-lipophilic balance (HLB) cartridge (4) 75 mg Z-sep, (5) 75 mg Z-sep+, (6) EMR-lipid cartridge, and (7) 50 mg ENVI-Carb) were compared. Due to its simplicity and cost-effectiveness, PRiME HLB was selected for clean-up. The recoveries of the target compounds were ranged from 86 to 96% with < 20% relative standard deviations. Therefore, this simple and effective method can be applied for the two pesticides and their metabolites in other edible insects or high-fat matrices.

Process Optimization of Ultrasound-assisted Enzyme Extraction of Biluochun Polysaccharide and Its Separation, Purification and Property Analysis

After the compound enzymatic hydrolysis of Biluochun tea powder, the ultrasonic-assisted extraction process of Biluochun polysaccharide (BTP) was optimized by response surface experiment. The anion column and gel column were used for separation and purification. The physicochemical composition, functional group composition, relative molecular mass and molecular conformation of each component were determined by Fourier transform infrared spectroscopy (FT-IR), ultraviolet spectrum scanning and high performance volume exclusion chromatography (HPSEC). The experiments showed that the best extraction process was ultrasonic power 200 W, ultrasonic temperature 45 ℃, material-to-liquid ratio 40:1 mL/g, ultrasonic time 35 min, and the yield of Biluochun polysaccharides was 26.74%. BTPA1 was obtained from BTP by DEAE-Sepharose anion exchange column chromatography, and BTPA1 was separated by Sepharose CL-6B gel column chromatography to obtain BTPA11 and BTPA12. The neutral sugar content of BTP, BTPA1, BTPA11 and BTPA12 were 59.39%, 66.86%, 77.43% and 62.61%, and the uronic acid content was 51.06%, 53.53%, 54.45% and 65.39%, respectively. After spectral and relative molecular mass analysis, the four Biluochun polysaccharide components all contained acid sugars and pyran ring structures; BTPA11 and BTPA12 were polysaccharides with uniform relative molecular mass distribution, and their relative molecular masses were 1604.2 kDa and 353.7 kDa; The slopes of the configuration of BTPA11 and BTPA12 were 0.12 and 0.15, and both might be high-branched spherical structures. The ultrasound-assisted enzyme extraction of Biluochun polysaccharide had a higher yield, and the analysis of the properties of each component would facilitate the study of fine structure and the development and utilization of active functions.

Feather protein lysate optimization and feather meal formation using YNDH protease with keratinolytic activity afterward enzyme partial purification and characterization

Incubation parameters used for the creation of a protein lysate from enzymatically degraded waste feathers using crude keratinase produced by the Laceyella sacchari strain YNDH were optimized using the Response Surface Methodology (RSM); amino acids quantification was also estimated. The optimization elevated the total protein to 2089.5 µg/ml through the application of the following optimal conditions: a time of 20.2 h, a feather concentration (conc.) of 3 g%, a keratinase activity of 24.5 U/100 ml, a pH of 10, and a cultivation temperature of 50 °C. The produced Feather Protein Lysate (FPL) was found to be enriched with essential and rare amino acids. Additionally, this YNDH enzyme group was partially purified, and some of its characteristics were studied. Crude enzymes were first concentrated with an Amicon Ultra 10-k centrifugal filter, and then concentrated proteins were applied to a "Q FF" strong anion column chromatography. The partially purified enzyme has an estimated molecular masses ranging from 6 to 10 kDa. The maximum enzyme activity was observed at 70 °C and for a pH of 10.4. Most characteristics of this protease/keratinase group were found to be nearly the same when the activity was measured with both casein and keratin-azure as substrates, suggesting that these three protein bands work together in order to degrade the keratin macromolecule. Interestingly, the keratinolytic activity of this group was not inhibited by ethylenediamine tetraacetic acid (EDTA), phenylmethanesulfonyl fluoride (PMSF), or iron-caused activation, indicating the presence of a mixed serine–metallo enzyme type.

Fractionation and structural characterization of polysaccharides derived from red grape pomace

Polysaccharides were recovered from red grape pomace by hot water extraction and then subjected to deproteinization, decolorization, fractionization, and characterization. The extraction process conferred a crude polysaccharide yield of 8.45 % (w/w) and the highest decolorization rate of 63.12 % was obtained by soaking the crude polysaccharide solution with 0.20 g/mL HPD-300 macroporous resin for 3 h. Separation with the anionic DEAE Fast Flow column generated four fractions, which were negatively charged according to zeta potential measurement. All the fractions contained uronic acid and their weight-average molecular weights were within the range 2 × 106–4 × 106 Dal. The most abundant fraction GPP-3 was composed of arabinose, xylose, mannose, glucose, and galactose in molar ratio 8.05:1.37:2.85:1.30:7.81 and rhamnose was also present according to FTIR and NMR analysis. AFM observation revealed that aggregation occurred in GPP-3, while the Congo red and β-elimination tests indicated the existence of triple helix and -O- linkage in the fraction. Hence, red grape pomace is a potential source of water-soluble polysaccharides and their bioactivity needs further study.

Hydroxylpyromorphite, a mineral important to lead remediation: Modern description and characterization

Abstract Hydroxylpyromorphite, Pb5(PO4)3(OH), has been documented in the literature as a synthetic and naturally occurring phase for some time but has not previously been formally described as a mineral. It is fully described here for the first time using crystals collected underground in the Copps mine, Gogebic County, Michigan. Hydroxylpyromorphite occurs as aggregates of randomly oriented hexagonal prisms, primarily between about 20–35 μm in length and 6–10 μm in diameter. The mineral is colorless and translucent with vitreous luster and white streak. The Mohs hardness is ~3½–4; the tenacity is brittle, the fracture is irregular, and indistinct cleavage was observed on {001}. Electron microprobe analyses provided the empirical formula Pb4.97(PO4)3(OH0.69F0.33Cl0.06)Σ1.08. The calculated density using the measured composition is 7.32 g/cm3. Powder X-ray diffraction data for the type material is compared to data previously reported for hydroxylpyromorphite from the talc mine at Rabenwald, Austria, and from Whytes Cleuch, Wanlockhead, Scotland. Hydroxylpyromorphite is hexagonal, P63/m, at 100 K, a = 9.7872(14), c = 7.3070(10) Å, V = 606.16(19) Å3, and Z = 2. The structure [R1 = 0.0181 for 494 F&amp;gt;4σ(F) reflections] reveals that hydroxylpyromorphite adopts a column anion arrangement distinct from other members of the apatite supergroup due to the presence of fluorine and steric constraints imposed by stereoactive lone-pair electrons of Pb2+ cations. The F– anion sites are displaced slightly from hydroxyl oxygen anions, which allows for stronger hydrogen-bonding interactions that may in turn stabilize the observed column-anion arrangement and overall structure. Our modern characterization of hydroxylpyromorphite provides deeper understanding to a mineral useful for remediation of lead-contaminated water.

Indigeneous Streptomyces spp. isolated from Cyperus rotundus rhizosphere indicate high mercuric reductase activity as a pontential bioremediation agent

Abstract. Rahayu HM, Putri WA, Khasanah AU, Sembiring L, Purwestri YA. 2021. Indigenous Streptomyces spp. isolated from Cyperus rotundus rhizosphere indicate high mercuric reductase activity as a potential bioremediation agent. Biodiversitas 22: 1519-1526. The purification and characterization of mercuric reductase of four indigenous Streptomyces spp. from Cyperus rotundus L. rhizosphere in mercury-contaminated area have been investigated. Cell-free extract was obtained by disrupting cells using sea sand at 4 °C followed by centrifugation. Mercuric reductase was purified by ammonium sulfate precipitation, dialysis, and chromatography column (DEAE Sepharose anion column chromatography). The determination of optimum pH and temperature of mercuric reductase activity was measured based on the number of NADPH2 oxidized to NADP per mg protein per minute using a spectrophotometer. The molecular weight of mercuric reductase was determined using SDS-PAGE. Result showed that the highest specific activity of mercuric reductase was recorded from Streptomyces spp. BR28. The optimum pH and temperature of cell-free extract enzyme mercuric reductase were 7.5 and 80 °C, respectively. The enzyme was purified to 431.87-fold with specific activity 21918.95 U/mg protein. SDS PAGE showed that the molecular weight of mercuric reductase in Streptomyces spp. BR 28 ranged from 50 kDa to 75 kDa. It can be concluded that Streptomyces isolates contain mercuric reductase and have potential as mercury bioremediation agent to overcome mercury contamination in the environment.

Production, partial purification and characterization of alkaline phosphatase from a thermo-alkaliphile Geobacillus thermodenitrificans I2 isolate

Abstract Alkaline phosphatases producing microbes are wide spread in nature; ALP is a hydrolase enzyme functioning at alkaline pH, able to hydrolyze phosphates from many types of molecules; this initiating many applications. Experimental designs were applied to evaluate the culture conditions affecting ALP production by Geobacillus thermodenitrificans strain I2, where glucose, yeast-extract and agitation were the most significant variables according to Plackett-Burman design (PBD). The optimum levels of these variables were assessed through Box–Behnken design (BBD) to be (g/L): glucose 26.4, yeast-extract 29.72 and agitation 150rpm, with a predicted enzyme activity of 8.149U/ml. The measured activity upon application the optimized medium was 7.896U/ml. Enzyme was partially purified (42%; 12 fold) through precipitation by ammonium sulfate and anion column, with two protein bands (>70 & ~40kDa) in SDS-PAGE. A partial gene translated sequence proved that the natively expressed ALP by studied strain is related to the band with ~40kDa. The partially purified enzyme exhibited maximum activity at 60°C and pH9.0, with remarkable temperature stability up to 65°C. The results indicated an enhancement in enzyme activity with metals (Mg2+, Mn2+) and reducing agents (DTT & s-mercaptoethanol) whereas, other metals (Zn2+, Hg2+), and anionic surfactant (SDS); EDTA; and PMSF inhibited the enzyme activity. The dependence on enzyme and substrate concentration was represented in Lineweaver-Burk plot where, Km and Vmax were 40mM and 25U/mg protein, respectively. In conclusion, the promising traits of studied ALP would underpin its efficient exploitation in several industries to cope with demands of worldwide enzyme markets.