Potentially Bioaccessible Phenolic and Antioxidant Potential of Fresh and Stored Lentil Sprouts—Effect of Lactobacillus plantarum 299v Enrichment

The phenolic and antioxidant potential of potentially bioaccessible fractions of lentil sprouts was studied. Sprouts were cocultivated with a probiotic to obtain a new functional product and further stored in cool conditions. The fraction obtained after buffer extraction and gastric digestion had higher content of phenolics compared to the control (by 20% and 46%, respectively); however, a 9% decrease was observed in samples obtained after gastrointestinal digestion. After gastrointestinal digestion, the highest content of phenolics (278 µg/g d.w.) was determined in the fresh control sprouts. Compounds neutralizing ABTS and hydroxyl radicals, chelating metal ions, and exhibiting strong reducing power were effectively released after gastrointestinal digestion (e.g., the values of the gastrointestinal digestibility index for chelating power and ability to quench hydroxyl radicals significantly exceeded 1 in all studied samples). It was proved that the enrichment of sprouts with a probiotic and further storage significantly improved the antioxidant potential; compared to the fresh control sprouts, an increase by 45% and 10% was determined after the gastric and gastrointestinal digestion, respectively. Lentil sprouts enriched with L. plantarum 299v may be a new functional product characterized by the high antioxidant capacity of the potentially bioaccessible fraction.     

Fractionation and Bioaccessibility of Manganese,Copper, Zinc,Cadmium, and Lead in Commercial Vegetable and Rice Baby Foods Using Inductively Coupled Plasma - Mass Spectrometry (ICP-MS) with Central Composite Design (CCD)

Abstract

Herein the bioaccessibility of Mn, Cu, Zn, Cd, and Pb, selected from essential and toxic elements, was determined in commercially sold vegetable purees intended for infant and toddler consumption. Chemical fractionation studies using water, acetone, diethyl ether, chloroform:methanol, and n-hexane were employed to predict the importance of the protein and lipid parts of a matrix to assess the bioaccessibility data. In addition, in-vitro gastrointestinal digestion was performed to determine the bioaccessibility of the elements using a five level, three factor central composite design (CCD) to maximize the elemental solubility. The total elemental concentrations in all of the fractions were determined by inductively coupled plasma – mass spectrometry (ICP-MS). Based on the consumption of one jar of vegetable/rice-based baby food, Zn was 1.3% of the recommended dietary allowance and Mn was 4.2% of the adequate intake level, while Cu was almost 100% of the adequate intake level. Additionally, Pb was always below the detection limit and Cd was sometimes under the detection limit for the percent bioaccessibility. However, in some samples, Cd was as high as 80% of the tolerable weekly intake level depending on the body weight.     

Separation of uranium from uraniferous coaly clays using a selective ion-exchange two-step elution system

Summary An ion-exchange process for the selective separation and enrichment of uranium from the main elements Si, Al, Fe, Ca, Mg, Na, K as well as from Mo and V, which are present in uraniferous coaly clays, has been developed. After a selective carbonate leaching of the roasted ore, a 0.5 mol/l Na₂CO₃/0.5 mol/l NaHCO₃ solution was passed through the macroporous ion-exchanger AG MP-1, which at pH10 absorbed uranium quantitatively in form of a carbonato complex. Remaining absorbed amounts of Mo and V were eluted with 0.1 mol/l EDTA in 0.5 mol/l Na₂CO₃/0.5 mol/l NaHCO₃, while U was quantitatively separated by a second elution step with 0.5 mol/l HNO₃ and was afterwards precipitated with NH₄OH as a high-grade yellow cake. Differential pulse polarography (DPP), atomic absorption spectroscopy (AAS), X-ray fluorescence (XRF), instrumental neutron activation analysis (INAA) and inductively coupled plasma mass spectrometry (ICP-MS) had been used to determine the uranium content in the raw materials and to investigate the effectivity of the different steps of the developed process.     

Study on multistage anodization for high-modulus carbon fiber

Because of the strong chemical inertness of high-modulus carbon fiber (HMCF), the surface treatment of HMCF becomes less effective. In this work, multistage anodization method was applied to modify HMCF. NH₄HCO₃ and (NH₄)₂SO₄ were used as electrolytes to study the influence of electrolyte type on the oxidation effect in the multistage oxidation process. The HMCF was treated by multistage anodization in the following three ways: NH₄HCO₃ → NH₄HCO₃, (NH₄)₂SO₄ → (NH₄)₂SO₄, and NH₄HCO₃ → (NH₄)₂SO₄. In order to compare with the multistage anodization methods, HMCF was also anodized by NH₄HCO₃ and (NH₄)₂SO₄ using single anodization method, respectively. The treated HMCFs were characterized in detail using X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, Scanning Electron Microscope (SEM), Atomic Force Microscope (AFM), and dynamic contact angle analysis, respectively. The results of XPS exhibited that HMCF modified by multistage anodization showed more functional groups on its surface. More sp2 hybridized bonds were converted into sp3 hybridized bonds after modification by multistage anodization, especially when (NH₄)₂SO₄ was used as electrolyte. The results of SEM/AFM indicated that HMCF modified by multistage showed a greater surface roughness. Interlaminar shear strength (ILSS) was used to observe the interfacial properties of HMCF between epoxy resin. The results showed that ILSS of untreated carbon fiber composite was only 27.3 MPa; it was increased to 71.8 and 78.6 MPa after treated with single anodization by NH₄HCO₃ and (NH₄)₂SO₄, respectively. After modification by multistage anodization, the ILSS increased in different degrees compared with single anodization method. Especially, the ILSS reached 93.1 MPa when the method of using NH₄HCO₃ followed by (NH₄)₂SO₄ was used to treat HMCF.     

Über die Identität eines sogenannten Ammoniumcarbonat‐Präparates

On the Identity of a so‐called Ammonium Carbonate Sample Commercial samples of so‐called “ammionum carbonate” are shown to contain ammonium carbamate rather than ammonium carbonate. In fact samples may contain varying quantities of α‐ and β‐(NH₄)(CO₂NH₂), of which only the α‐phase is reported in the literature. Mixtures of both phases tend to leak the volatile α‐phase and to react with moisture to form (NH₄)(HCO₃). The crystal structure of the new β‐(NH₄)(CO₂NH₂) is refined from X‐ray powder data.     

High electrochemical activity of Pt/C cathode modified with NH4HCO3 for direct methanol fuel cell

The electrochemical activity of Pt/C cathode for direct methanol fuel cell was improved by introducing NH₄HCO₃ to the catalyst layer as the pore-forming agent during preparation process of catalyst-coated membrane. SEM analysis revealed that NH₄HCO₃ contributed to the formation of additional porosity and the dispersion of the catalyst particles. The modified catalyst layer promoted the electrochemical and mass transport processes. It was suggested that the optimal weight ratio of the catalyst to NH₄HCO₃ was 2:3. As a result, the single cell exhibited a 21% increment in the peak power density at 50 °C, with a highest electrochemical surface area of 446 cm² mg_Pt^–1. However, an extremely high content of NH₄HCO₃ yielded discontinuous pathways for the electron transfer in the catalyst layer.     

Influence of digestion methods on the determination of total Al in food samples by ICP-ES

Summary To determine total Al in a variety of food and total diet samples using ICP-ES, HF pre-treatment, prior to wet digestion (HNO₃/HClO₄) seems to be necessary. Compared with results obtained after HF pre-treatment, the determination of Al using pressure microwave digestion with HNO₃ or HNO₃/HClO₄ digestion recovered only between 25–50% Al for dried spinach and flour and 40–75% for total diet samples, respectively. In most cases the addition of 0.25 ml HF (40%) per gram dry mass resulted in maximum Al yield. The results are in acceptable agreement with those obtained by neutron activation analysis (NAA).     

Determination of Arsenic,Cadmium, Cobalt,Chromium, Nickel,and Lead in Cosmetic Face-Powders: Optimization of Extraction and Validation

An analytical method for the quantification of toxic metals in face-powders is presented and discussed. Acid digestion with HNO₃-H₂O₂ or HNO₃-HCl was performed and compared with total digestion by HF. The digestion with HNO₃-H₂O₂ was the most suitable for these purposes. Analyses were performed by inductively coupled plasma atomic emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS), whose performances were compared by analyzing three different certified reference materials. The analysis of five commercial face-powders revealed the presence of all the considered metals in the range 0.06–8.0 µg/g. To simulate the bioaccessibility of metals in physiological conditions, a digestion with a simulated sweat solution was performed. In this case, the analysis of the same face-powder samples provided results below the limit of quantification, suggesting low bioaccessibility of the considered trace elements.     

Effect of weak base modification on ZSM‐5 catalyst for methanol to aromatics

The effect of weak base modification on the catalytic performance of ZSM‐5 catalyst for conversion of methanol to aromatics was investigated. The catalysts were characterized using X‐ray diffraction, X‐ray fluorescence, N₂ adsorption–desorption, NH₃ temperature‐programmed desorption, Fourier transform infrared spectroscopy, scanning electron microscopy and thermogravimetry. The results showed that catalysts treated with weak base (NaHCO₃, Na₂CO₃ and NH₃⋅H₂O) exhibited a pore structure with interconnected micropores and mesopores. The existence of mesopores was beneficial for improving the diffusion of reactants and products, and the coke deposition resistance capacity of treated catalysts was enhanced greatly. Meanwhile, compared to traditional ZSM‐5 zeolite, the ratio of Brønsted to Lewis (B/L) acid sites of ZSM‐5/NH₃⋅H₂O (B/L = 7.35) zeolite slightly increased but the amount of acid sites reduced, while those of ZSM‐5/NaHCO₃ (B/L = 0.127) and ZSM‐5/Na₂CO₃ (B/L = 0.107) significantly reduced. Further, the catalyst treated with NH₃⋅H₂O solution was evaluated in the methanol to aromatics reaction and led to an enhanced aromatization reaction rate. The liquid hydrocarbons product distribution exhibited higher aromatic hydrocarbons yield (56.12%) and selectivity (40.28%) of benzene, toluene and xylene (BTX) with isoparaffin content reducing to 26.17%, which could be explained by appropriate B/L acid sites ratio, higher pore volumes and higher surface area.     

Analysis of bioaccessible concentration of trace elements in plant based edible materials by INAA and ICPMS methods

The total metal concentration and bioaccessible concentration of Cr, Mn, Fe, Cu, Zn, Se in Momordica charantia, Asparagus racemosus, Terminalia arjuna and Syzyzium cumini were measured by instrumental neutron activation analysis and by inductively coupled plasma mass spectrometry analysis (ICP-MS). The bioaccessible concentrations were determined in the gastrointestinal digest obtained after treating dried powdered samples sequentially in gastric and intestinal fluid of porcine origin at physiological conditions. The bioaccessible concentration of Fe was in the range of 58–67 mg kg^?1, Mn was 10.2–14.6 mg kg^?1, Cu was 3.7–4.8 mg kg^?1 and Zn was 10.6–18.4 mg kg^?1, were within the safety limits set for vegetable food stuff set by Joint FAO/WHO. The bioaccessibility of Zn, an essential element, was high (40–50 %) in M. charantia and in S. cumini. In addition, the total metal contents and bioaccessible concentration of Ni, Se, Cd and Pb in these samples were measured by ICP-MS. The total Cd content in S. cumini (2.6 ± 0.2 mg kg^?1) and its bioaccessible concentration (0.6 mg kg^?1) were strikingly high as compared to the other samples. Though total Hg contents were determined by ICP-MS, but their bioaccessible concentrations were below the detection limit (0.036 mg kg^?1).     

The study on the preparation methods and the fluidity of large rare earth oxide particles

In this work large CeO₂ particles were prepared using H₂C₂O₄ and NH₄HCO₃ as precipitators. The effects of feeding mode and speed, stirring speed, aging time, precipitate and calcination temperature and precipitation method on physicochemical properties of CeO₂ were studied when the precipitator was H₂C₂O₄. By the NH₄HCO₃ precipitation method, the effects of adding inoculating crystals and additives on particle size, loose density and fluidity of CeO₂ were investigated. Under optimized conditions, large CeO₂ particles with high loose density and good fluidity of can be prepared by either H₂C₂O₄ or NH₄HCO₃ precipitation method. SEM also investigates the morphology of the particles prepared by both methods. The results show that physicochemical properties of CeO₂ particles prepared by the NH₄HCO₃ precipitation method are not as good as those of CeO₂ particles prepared by the H₂C₂O₄ precipitation method. However, both methods are suitable for industrial production due to their simple processes, low equipment investment and ease for industrial development. Our results show that large rare earth particle can be prepared by the optimized conventional methods. This study provided a useful method to prepare of large rare earth particles.     

Mean activity coefficients in the NaCl–NH4HCO3–H2O system at 293.15–308.15 K

The mean activity coefficients of NaCl in the NaCl–NH₄HCO₃–H₂O system, measured by an electrochemical cell using ion-selective electrodes, were used to calculate the mean activity coefficients of NH₄HCO₃ in the system through a thermodynamic model. The measurements were made at four temperatures from 293.15 to 308.15 K up to 1.8 mol kg⁻¹, at NH₄HCO₃ molality fractions of 0.2 and 0.4. Both sets of values agree with those obtained from Pitzer equation incorporated with chemical reactions. This observation supports the applicability of the existing parameters for calculating mean activity coefficients of this system.     

Testing the retardancy effect of various inorganic chemicals on smoldering combustion of Pinus halepensis needles

The fire retarding performance of 28 different inorganic chemical substances was tested by measuring the relative particle fire hazard properties of Pinus halepensis needles treated with these chemicals. The tests were performed using a new method, based on a specifically designed apparatus for monitoring the forest species temperature, under precisely controlled temperature and static air atmosphere conditions. The relative ignition and smoldering combustion properties determined were: the ignition delay time, the combustion rate, the heat content and the mass residue of forest samples. The key elements for the effectiveness of fire retardants were the delay of ignition and the reduction of heat and combustion rate. The chemicals examined were: Cu, Fe, Al₂O₃, Fe₂O₃, SiO₂·H₂O, NaHCO₃, KI, KBr, KCl, NaCl, CaCO₃, MnSO₄·5H₂O, CuSO₄·5H₂O, MgCl₂·6H₂O, Na₂B₄O₇·10H₂O, Na₂HPO₄, Na₂CO₃, Na₂SiO₃, ZnSO₄·7H₂O, Zn₃(PO₄)₂·2H₂O, NH₄Br, NH₄Cl, NH₄HCO₃, (NH₄)₂CO₃, NH₄H₂PO₄ (MAP), (NH₄)₂SO₄ (AS), (NH₄)₂HPO₄ (DAP) and a commercial retardant containing both DAP and AS. Among them the best performance was exhibited by ammoniac phosphates, followed by ammoniac sulfates and silica.     

Assessment of a geochemical extraction procedure to determine the solid phase fractionation and bioaccessibility of potentially harmful elements in soils: A case study using the NIST 2710 reference soil

Three mineral acid sequential extraction regimes (HNO₃ only, HNO₃ followed by HCl and aqua regia) were applied to the NIST 2710 contaminated reference soil. The major and trace element chemical analysis data from the extractions were subjected to a chemometric self-modelling mixture resolution procedure which identified that 12 distinct physico-chemical components were extracted. The fractionation of As, Cd, Ni and Pb between these components were determined. Tentative assignments of the mineralogical sources of the components were made. The human ingestion bioaccessible fraction of As, Cd and Pb were determined using the in vitro BARGE UBM bioaccessibility test and were found to be 51.6%, 68.0% and 68.4% respectively. The relationship between the lability of the physico-chemical components and the bioaccessible fraction of the soils was investigated and the bioaccessible fractions were assigned to specific components. The extraction scheme using aqua regia was found to be the most suitable as it was the only one which extracted the iron sulphide phase in the soil.     

Improvement of gel‐separated protein identification by DMF‐assisted digestion and peptide recovery after electroblotting

In‐gel digestion of gel‐separated proteins is a major route to assist in proteomics‐based biological discovery, which, however, is often embarrassed by its inherent limitations such as the low digestion efficiency and the low recovery of proteolytic peptides. For overcoming these limitations, many efforts have been directed at developing alternative methods to avoid the in‐digestion. Here, we present a new method for efficient protein digestion and tryptic peptide recovery, which involved electroblotting gel‐separated proteins onto a PVDF membrane, excising the PVDF bands containing protein of interest, and dissolving the bands with pure DMF (≥99.8%). Before tryptic digestion, NH₄HCO₃ buffer was added to moderately adjust the DMF concentration (to 40%) in order for trypsin to exert its activity. Experimental results using protein standards showed that, due to actions of DMF in dissolving PVDF membrane and the membrane‐bound substances, the proteins were virtually in‐solution digested in DMF‐containing buffer. This protocol allowed more efficient digestion and peptide recovery, thereby increasing the sequence coverage and the confidence of protein identification. The comparative study using rat hippocampal membrane‐enriched sample showed that the method was superior to the reported on‐membrane tryptic digestion for further protein identification, including low abundant and/or highly hydrophobic membrane proteins.     

Development and applications of <Emphasis Type="Italic">k</Emphasis><Subscript>0</Subscript> based NAA and prompt gamma-ray NAA methods at BARC

A summary of k ₀-based R&D work on neutron activation analysis (NAA), internal mono standard NAA (IM-NAA) and prompt gamma-ray NAA (PGNAA) is presented. The k ₀-based NAA was standardized by characterizing irradiation sites of research reactors, validated using reference materials and applied to samples of different origin. Recently IM-NAA method was developed, validated for small and large size samples and applied for the analysis of large size as well as non-standard geometry samples. Studies on PGNAA included characterization of neutron beam, determinations of detection efficiency and prompt k ₀-factors, and analytical applications.     

A modified lead–matrix separation procedure shown for lead isotope analysis in Trojan silver artefacts as an example

A modified Pb–matrix separation procedure using NH₄HCO₃ solution as eluent has been developed and validated for determination of Pb isotope amount ratios by thermal ionization mass spectrometry. The procedure is based on chromatographic separation using the Pb·Spec resin and an in-house-prepared NH₄HCO₃ solution serving as eluent. The advantages of this eluent are low Pb blanks (<40 pg?mL^?1) and the property that NH₄HCO₃ can be easily removed by use of a heating step (>60 °C). Pb recovery is >95 % for water samples. For archaeological silver samples, however, the Pb recovery is reduced to approximately 50 %, but causes no bias in the determination of Pb isotope amount ratios. The validated procedure was used to determine lead isotope amount ratios in Trojan silver artefacts with expanded uncertainties (k?=?2) <0.09 %.     

Dynamic continuous-flow dialysis method to simulate intestinal digestion for in vitro estimation of mineral bioavailability of food

A system for dynamic continuous-flow dialysis during intestinal digestion for an in vitro simulation of gastrointestinal digestion is presented as an alternative to human and animal in vivo methods for estimation of the bioavailability of minerals. The method is based on the in vitro batch dialysis method described by Miller, which was developed into a continuous-flow system of a simple design to perform dynamic dialysis in the intestinal digestion stage. A flow dialysis system has the advantages of simulation being close to in vivo physiological conditions because pH change during dialysis is gradual and dialyzed components are continuously removed. The proposed new design performed dialysis during a continuous flow of dialyzing solution (NaHCO₃) around a dialysis bag containing peptic digest, which is placed inside a glass dialysis chamber. Gradual change of dialysis pH, similar to that occurring in the gastrointestinal tract, was obtained by optimization of flow rate and concentration of NaHCO₃. The dialysate collected in fractions was analyzed to determine dialyzed minerals and pH change in the course of dialysis. The method was tested by determination of calcium bioavailability of powder milk and calcium carbonate tablets.     

The “Borrowing Hydrogen Strategy” by Supported Ruthenium Hydroxide Catalysts: Synthetic Scope of Symmetrically and Unsymmetrically Substituted Amines

The N‐alkylation of ammonia (or its surrogates, such as urea, NH₄HCO₃, and (NH₄)₂CO₃) and amines with alcohols, including primary and secondary alcohols, was efficiently promoted under anaerobic conditions by the easily prepared and inexpensive supported ruthenium hydroxide catalyst Ru(OH)_x/TiO₂. Various types of symmetrically and unsymmetrically substituted “tertiary” amines could be synthesized by the N‐alkylation of ammonia (or its surrogates) and amines with “primary” alcohols. On the other hand, the N‐alkylation of ammonia surrogates (i.e., urea and NH₄HCO₃) with “secondary” alcohols selectively produced the corresponding symmetrically substituted “secondary” amines, even in the presence of excess amounts of alcohols, which is likely due to the steric hindrance of the secondary alcohols and/or secondary amines produced. Under aerobic conditions, nitriles could be synthesized directly from alcohols and ammonia surrogates. The observed catalysis for the present N‐alkylation reactions was intrinsically heterogeneous, and the retrieved catalyst could be reused without any significant loss of catalytic performance. The present catalytic transformation would proceed through consecutive N‐alkylation reactions, in which alcohols act as alkylating reagents. On the basis of deuterium‐labeling experiments, the formation of the ruthenium dihydride species is suggested during the N‐alkylation reactions.     

Iron-catalyzed hydroaminocarbonylation of alkynes: Selective and efficient synthesis of primary α,β-unsaturated amides

α,β-Unsaturated primary amides are important intermediates and building blocks in organic synthesis. Herein, we report a ligand-free iron-catalyzed hydroaminocarbonylation of alkynes using NH₄HCO₃ as the ammonia source, enabling the highly efficient and regioselective synthesis of linear α,β-unsaturated primary amides. Various aromatic and aliphatic alkynes are transformed into the desired linear α,β-unsaturated primary amides in good to excellent yields. Further studies show that using NH₄HCO₃ as the ammonia source is key to obtain good yields and selectivity. The utility of this route is demonstrated with the synthesis of linear α,β-unsaturated amides including vanilloid receptor-1 antagonist TRPV-1.