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1.
Food Chem ; 457: 140032, 2024 Jun 12.
Artigo em Inglês | MEDLINE | ID: mdl-38936117

RESUMO

The aim of the presented study was to evaluate the release of the enzymatically initiated production of hexanal from double emulsion electrospun bio-active membranes at a temperature of fruit storage. Among different formulations of water-in-oil (W1/O) primary emulsions, the emulsion composed of 12% w/v Tween20 and 0.1 M NaCl in water (W1) and 6% of poly(glycerol) poly(ricinoleate) dissolved in sunflower oil (O) using W1/O ratio of 80/20 (w/w) (Tween20-NaCl/6% PGPR) was selected, for further incorporation of enzymes, based on the lowest average droplet size (391.0 ± 15.6 nm), low polydispersity index (0.255 ± 0.07), and good gravitational stability also after 14 days. Both enzymes, lipase and lipoxygenase are needed to produce hexanal (up to 58 mg/L). Additionally, double emulsions were prepared with sufficient conductivity and viscosity using different W1/O to W2 ratios for electrospinning. From the selected electrospun membrane, up to 4.5 mg/L of hexanal was released even after 92 days.

2.
Environ Geochem Health ; 45(12): 9855-9873, 2023 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-37864130

RESUMO

Acid mine drainage (AMD) is generally outlined as one of the largest environmental concerns, characterized by very low pH value of mine waste, heavy metals and high sulphate content. This extremely hostile environment reduces plant ability to develop and grow. Present study focuses on a silver birch (Betula pendula Roth), a pioneer species that grows on an extremely hostile gold mine waste, to investigate the bioaccumulation of rare metals (thallium (Tl) and indium (In)), as well as nine other more common heavy metals (bismuth (Bi), cadmium (Cd), cobalt (Co), copper (Cu), lead (Pb), manganese (Mn), nickel (Ni), silver (Ag) and zinc (Zn)), and to asses phytoextraction and phytostabilization potential of silver birch. Additionally, parameters determining AMD process and overall contamination (pH, electrical conductivity (EC), sulphates (SO42-), arsenic (As), iron (Fe), oxidation-reduction potential (ORP), turbidity, dissolved oxygen (DO), total dissolved solids (TDS), acidity, hardness, X-ray diffraction (XRD) and radioactivity) were determined in mine waste and drainage water samples. To assess the heavy metals bioaccumulation and mine waste status, statistical geochemical indices were determined: bioaccumulation factor (BCF), pollution load index (PLI), geochemical abundance index (GAI) and exposure index (EI). The results show that silver birch bioaccumulates the essential elements Cu, Ni, Mn and Zn, and the nonessential elements Tl (average BCF = 24.99), In (average BC = 23.01) and Pb (average BCF = 0.84). Investigated mine waste was enriched by Bi, Ag and Cd according to positive values of GAI index. Present research provides a novel insight into bioaccumulation of nonessential heavy metals in silver birches who grow on the extremely hostile mine waste, and they exhibit significant phytoremediation potential.


Assuntos
Betula , Metais Pesados , Ouro , Cádmio , Bioacumulação , Chumbo , Metais Pesados/análise , Zinco , Manganês , Monitoramento Ambiental
3.
Mar Pollut Bull ; 196: 115665, 2023 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-37866053

RESUMO

This study investigated the contents of macrominerals (Na, K, Ca, Mg and P) and essential trace metals (Fe, Mn, Cu, Zn and Se) in four species of seaweeds (Gracilaria sp., Alsidium corallinum, Caulerpa prolifera, and Chaetomorpha sp.) from Marchica Lagoon. The contents of macrominerals with mean values (% dw) can be sequenced in this descending order, [Ca > Mg > Na > K > P] for Caulerpa prolifera, and the decreasing sequence [K > Ca > Mg > P > Na] for Chaetomorpha sp. In red seaweeds, Gracilaria sp. and Alsidiumcorallinum followed these orders: [K > Ca > Na > Mg > P] and [K > Na > Ca > Mg > P] respectively. The essential trace metals mean values (mg kg-1) followed the decreasing order [Fe > Mn > Zn > Cu > Se] for Alsidiumcorallinum, Chaetomorpha sp. and Gracilaria sp., and the following order [Fe > Mn > Zn > Se > Cu] for Caulerpa prolifera. Based on the calculated recommended dietary allowance (RDA), targeted hazard quotient (THQ) and the hazard index (HI), the studied seaweeds did not pose any health risk for human consumption.


Assuntos
Caulerpa , Clorófitas , Gracilaria , Alga Marinha , Oligoelementos , Humanos , Mar Mediterrâneo , Oligoelementos/análise , Medição de Risco , Valor Nutritivo
4.
Plants (Basel) ; 12(16)2023 Aug 08.
Artigo em Inglês | MEDLINE | ID: mdl-37631102

RESUMO

Polyphenols from Slovenian hops (Humulus lupulus L.) of the Aurora variety were extracted by different methods and using classical solvents and several deep eutectic solvents (DES) based on choline chloride as the hydrogen bond acceptor component. The obtained extract solutions were analyzed by HPLC for the content of extracted α- and ß-acids and extracted xanthohumol. It was found that choline chloride:phenol DES concentrated aqueous solution had an extraction efficiency close to that of diethyl ether, which is considered one of the best classical extraction solvents for polyphenols from hops. The comparison of the extraction efficiency with other choline chloride-based DESs showed that the chemical similarity of the phenol ring in the solvent DES with the polyphenols in hops may be crucial for a highly efficient extraction with choline chloride:phenol DES. On the other hand, the choice of extraction method and the viscosity of the solvents tested seem to play only a minor role in this respect. As far as we know, this is the first study to attempt to relate extraction efficiency in the extraction of hydrophobic solutes to the compressibility of the DES extractants, the latter of which may be correlated with the extent of hydrophobic hydration around the DES components. In addition, using the heating and stirring method for the preparation of choline chloride-based DES concentrated aqueous solutions we found no support for the occurrence of water in two different roles (in the structural and in the dilution role) in these solvents.

5.
Foods ; 12(15)2023 Jul 25.
Artigo em Inglês | MEDLINE | ID: mdl-37569095

RESUMO

In the present study, the potential of elemental analysis combined with statistical tools to identify honey origin was evaluated by mineral characterization of 173 honeys of 13 floral types (acacia, fir, spruce, linden, chestnut, lavender, coriander, thistle, honeydew, rosemary, sage, euphorbia and ziziphus plant species) collected from five geographical regions (Slovenia, Croatia, Bulgaria, Turkey, and Morocco). The objective of the study was to accurately and reliably differentiate the mineral composition among honey varieties. The aim was to establish traceability, to ensure product authenticity and to improve quality control measures within the honey industry. For this purpose, 18 major, minor and trace elements were quantified using microwave digestion, followed by ICP-MS measurement. Statistical evaluation of elemental concentration was undertaken using principal component analysis (PCA) to distinguish honey floral types. The research give light on the specific elements that can serve as indicators for determining the geographical and botanical source of honey. Our findings indicate that certain elements, such as Mn, K, and Ca, are primarily influenced by the type of pollen present in the honey, making them indicative of the floral source. On the other hand, levels of Na, Mg, and Fe were found to be more strongly influenced by environmental factors and can be considered as markers of geographical origin. One novel aspect of this research is the exploration of the relationship between honey minerals and honey botanical source. This was achieved through the analysis of chestnut tree samples and a subsequent comparison with the composition of chestnut honey.

6.
Sensors (Basel) ; 22(23)2022 Nov 26.
Artigo em Inglês | MEDLINE | ID: mdl-36501902

RESUMO

Potentiometry with membrane selective electrodes is preferable for measuring the various constituents of pharmaceuticals. In this work, carbon paste electrodes (CPE) were prepared, modified, and tested for the determination of maprotiline hydrochloride, which acts as an antidepressant. The proposed CPE was based on an ionic association complex of maprotiline-tetraphenylborate, 2-nitrophenyloctyl as a binder, and sodium tetraphenylborate as an ionic lipophilic additive. The optimized composition improved potentiometric properties up to theoretical Nernst response values of -59.5 ± 0.8 mV dec-1, in the concentration range of maprotiline from 1.6 × 10-7 to 1.0 × 10-2 mol L-1, and a detection limit of 1.1 × 10-7 mol L-1. The CPE provides excellent reversibility and reproducibility, exhibits a fast response time, and is applicable over a wide pH range. No significant effect was observed in several interfering species tested. The proposed electrode was used for the precise determination of maprotiline in pure solutions, urine samples, and a real sample-the drug Ludiomil.


Assuntos
Carbono , Maprotilina , Carbono/química , Reprodutibilidade dos Testes , Potenciometria , Preparações Farmacêuticas
7.
Sensors (Basel) ; 22(24)2022 Dec 07.
Artigo em Inglês | MEDLINE | ID: mdl-36559958

RESUMO

A simple, sensitive, cost effective, and reliable enzymatic glucose biosensor was developed and tested. Nitrogen-doped heat-treated graphene oxide nanoribbons (N-htGONR) were used for modification of commercially available screen-printed carbon electrodes (SPCEs), together with MnO2 and glucose oxidase. The resulting sensors were optimized and used to detect glucose in a wide linear range (0.05-5.0 mM) by a simple amperometric method, where the limit of detection was determined to be 0.008 mM. (lifetime), and reproducibility studies were also carried out and yielded favorable results. The sensor was then tested against potential interfering species present in food and beverage samples before its application to real matrix. Spiked beer samples were analyzed (with glucose recovery between 93.5 and 103.5%) to demonstrate the suitability of the developed sensor towards real food and beverage sample applications.


Assuntos
Técnicas Biossensoriais , Grafite , Nanotubos de Carbono , Reprodutibilidade dos Testes , Compostos de Manganês , Óxidos , Técnicas Eletroquímicas/métodos , Glucose , Eletrodos , Técnicas Biossensoriais/métodos
8.
ACS Appl Energy Mater ; 5(8): 9571-9580, 2022 Aug 22.
Artigo em Inglês | MEDLINE | ID: mdl-36034758

RESUMO

Graphene derivatives doped with nitrogen have already been identified as active non-noble metal materials for oxygen reduction reaction (ORR) in PEM and alkaline fuel cells. However, an efficient and scalable method to prepare active, stable, and high-surface-area non-noble metal catalysts remains a challenge. Therefore, an efficient, potentially scalable strategy to improve the specific surface area of N-doped graphene derivatives needs to be developed. Here, we report a novel, rapid, and scalable electrical induction heating method for the preparation of N-doped heat-treated graphene oxide derivatives (N-htGOD) with a high specific surface area. The application of the induction heating method has been shown to shorten the reaction time and improve the energy efficiency of the process. The materials synthesized by induction heating exhibited very high specific surface area and showed improved ORR activity compared to the conventional synthesis method. Moreover, we demonstrated that the temperature program of induction heating could fine-tune the concentration of nitrogen functionalities. In particular, the graphitic-N configuration increases with increasing final temperature, in parallel with the increasing ORR activity. The presented results will contribute to the understanding and development of nonmetal N-htGOD for energy storage and conversion applications.

9.
Materials (Basel) ; 15(12)2022 Jun 17.
Artigo em Inglês | MEDLINE | ID: mdl-35744361

RESUMO

Sedimentation is a naturally occurring process of allowing particles in water bodies to settle out of the suspension under a gravity effect. In this study, the sediments of the Drava River were fully investigated to determine the heavy metal concentrations along the river and their potential reuse in the construction sector. Naturally dehydrated sediments from the Drava River were tested as an additive for the production of fired bricks. The dredged sediments were used as a substitute for natural brick clay in amounts up to 50% by weight, and it was confirmed that up to 20% by weight of the added sediment could be used directly in the process without critically affecting performance. Finally, the naturally dehydrated sediments were also evaluated for their use as a filling material in the construction of levees. The natural moisture content of the dehydrated sediment was too high for it to be used without additives, so quicklime was added as an inorganic binder. The test results showed an improvement in the geotechnical properties of the material to such an extent that it is suitable as a filling material for levees.

10.
ACS Omega ; 7(15): 12610-12616, 2022 Apr 19.
Artigo em Inglês | MEDLINE | ID: mdl-35474763

RESUMO

Palladium was immobilized on a highly porous copolymer of 4-vinylpyridine and divinylbenzene (polyHIPE-poly(high internal phase emulsion)) using palladium(II) acetate to obtain PolyPy-Pd with 6.1 wt % or 0.57 mmol Pd/g. The immobilized catalyst was able to catalyze the coupling of iodobenzene and phenylboronic acid in ethylene glycol monomethyl ether/water (3:1) within 4 h at rt and complete conversion was observed when 2.5 mol % of Pd per PhI was used. The reaction tolerated a wide range of substituents on the aromatic ring. Iodobenzene derivatives with electron-withdrawing substituents showed higher reactivity, while the opposite was true for the phenylboronic acid series. The polyHIPE-supported Pd catalyst was also used for the direct conversion of phenylboronic acid to biphenyl through an iodination/coupling reaction sequence. The recyclability of the heterogeneous catalyst was also optimized, and by finding a suitable combination of solvents for the loading of Pd, the reaction, and the isolation of the product, the solid-supported catalyst was completely regenerated and used in the next reaction with the same activity.

11.
Antioxidants (Basel) ; 11(4)2022 Apr 06.
Artigo em Inglês | MEDLINE | ID: mdl-35453409

RESUMO

In this study, the extraction efficiency of natural deep eutectic solvents (NADES) based on choline chloride as a hydrogen bond acceptor (HBA) and five different hydrogen bond donors (HBD; lactic acid, 1,4-butanediol, 1,2-propanediol, fructose and urea) was evaluated for the first time for the isolation of valuable bioactive compounds from Achillea millefolium L. The phytochemical profiles of NADES extracts obtained after ultrasound-assisted extraction were evaluated both spectrophotometrically (total phenolic content (TPC) and antioxidant assays) and chromatographically (UHPLC-MS and HPLC-UV). The results were compared with those obtained with 80% ethanol, 80% methanol, and water. The highest TPC value was found in the lactic acid-based NADES (ChCl-LA), which correlated with the highest antioxidant activity determined by the FRAP analysis. On the other hand, the highest antiradical potential against ABTS+• was determined for urea-based NADES. Phenolic acids (chlorogenic acid and dicaffeoylquinic acid isomers), flavones (luteolin and apigenin), and their corresponding glucosides were determined as the dominant individual phenolic compounds in all extracts. The antibacterial and antifungal properties of the extracts obtained against four bacterial cultures and two yeasts were evaluated using two methods: the agar dilution method to obtain the minimum inhibitory concentration (MIC) and the minimum bactericidal or fungicidal concentration (MBC or MFC), and the disc diffusion method. ChCl-LA had the lowest MIC and MBC/MFC with respect to all microorganisms, with an MIC ranging from 0.05 mg mL-1 to 0.8 mg mL-1, while the water extract had the weakest inhibitory activity with MIC and MBC/MFC higher than 3.2 mg mL-1.

12.
J Vasc Access ; 23(4): 543-549, 2022 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-33752479

RESUMO

BACKGROUND: Citrate is instilled into the dialysis catheter to prevent clotting and to maintain patency between dialysis sessions. A significant amount of citrate leaks from the catheter at the injection time, which decreases the blood ionized calcium concentration (Ca2+) due to chelation. We aimed to evaluate the local impact of concentrated (i.e. 30%) citrate spilling on Ca2+ at the catheter tip in real-time pediatric conditions. METHODS: An in-vitro model was constructed, involving an ion-selective electrode (Ca-ISE). A pre-curved catheter and the Ca-ISE were submerged in a glass vessel with the tips positioned adjacent to each other. The vessel was filled with 30 and 80 ml of normal saline with added calcium to simulate normal right atrium size in children and adults, respectively, and normal blood Ca2+. The amount of instilled citrate matched the filling volume of the catheter. Measurements were performed with 4% and 30% citrate solutions. RESULTS: The mean Ca2+ measured at the tip of the catheter was 0.457 and 0.058 mmol/l when using 4% and 30% citrate, respectively (p < 0.001). The mean Ca2+ recorded in 30 and 80 ml after instilling 30 % citrate was 0.058 and 0.055 mmol/l, respectively (p = 0.878). CONCLUSIONS: The spilling of 30% citrate caused a strikingly greater decrease of Ca2+ at the catheter tip than the standard 4% citrate. The atrial volume did not influence the test results implying similar safety concerns for pediatric and adult patients. The used static experimental setting might have overestimated the spilling effect.


Assuntos
Cálcio , Ácido Cítrico , Adulto , Anticoagulantes/efeitos adversos , Criança , Citratos , Humanos , Diálise Renal/métodos
13.
Sensors (Basel) ; 21(24)2021 Dec 11.
Artigo em Inglês | MEDLINE | ID: mdl-34960395

RESUMO

Four different graphene-based nanomaterials (htGO, N-htGO, htGONR, and N-htGONR) were synthesized, characterized, and used as a modifier of carbon paste electrode (CPE) in order to produce a reliable, precise, and highly sensitive non-enzymatic amperometric hydrogen peroxide sensor for complex matrices. CPE, with their robustness, reliability, and ease of modification, present a convenient starting point for the development of new sensors. Modification of CPE was optimized by systematically changing the type and concentration of materials in the modifier and studying the prepared electrode surface by cyclic voltammetry. N-htGONR in combination with manganese dioxide (1:1 ratio) proved to be the most appropriate material for detection of hydrogen peroxide in pharmaceutical and saliva matrices. The developed sensor exhibited a wide linear range (1.0-300 µM) and an excellent limit of detection (0.08 µM) and reproducibility, as well as high sensitivity and stability. The sensor was successfully applied to real sample analysis, where the recovery values for a commercially obtained pharmaceutical product were between 94.3% and 98.0%. Saliva samples of a user of the pharmaceutical product were also successfully analyzed.


Assuntos
Grafite , Nanotubos de Carbono , Carbono , Técnicas Eletroquímicas , Eletrodos , Peróxido de Hidrogênio , Limite de Detecção , Compostos de Manganês , Óxidos , Reprodutibilidade dos Testes , Saliva
14.
Antibiotics (Basel) ; 10(11)2021 Nov 17.
Artigo em Inglês | MEDLINE | ID: mdl-34827345

RESUMO

Amoxicillin (AMX) and Ciprofloxacin (CIP) are antibiotics commonly used in human medicine with high environmental toxicity and poor biodegradability. They have been found in various hospital effluents and groundwater, and their environmental impact is still not fully understood. In this work, we investigated the possibility of treating model wastewaters containing the antibiotics AMX and CIP using ozonation, with the addition of H2O2 under various conditions, including different pH values, H2O2, and ozone dosages. The quantification of and treatment efficacy for antibiotic removal were determined via solid phase extraction followed by chromatographic separation by liquid chromatography coupled with tandem triple quadrupole mass spectrometry (LC/MS/MS). This analytical system is quite efficient for the detection of all major antibiotic classes, even if they are present at very low concentrations. The efficiency of ozonation was determined by measuring the TOC (Total Organic Carbon) changes after ozonation of the model wastewater and by measuring the concentration of the two antibiotics. In a sequential activated sludge process of ozone-treated model wastewater, almost complete TOC removal and an overwhelming decrease in antibiotic concentrations (up to 99%) were observed. Ozonation resulted in complete removal of AMX and CIP in less than 30 and 120 min, respectively. The results of this work indicate that ozonation could be a suitable pretreatment method to reduce the toxicity of contaminants (AMX and CIP) and improve the biodegradability of hospital wastewater.

15.
Polymers (Basel) ; 13(16)2021 Aug 14.
Artigo em Inglês | MEDLINE | ID: mdl-34451260

RESUMO

With the aim to study the influence of monomer ratio in poly(high internal phase emulsions) (polyHIPEs) on the polymer network architecture and morphology of poly(vinylbenzyl chloride-co-divinylbenzene-co-styrene) after hypercrosslinking via the internal Friedel-Crafts process, polyHIPEs with 80% overall porosity were prepared at three different initial crosslinking degrees, namely 2, 5, and 10 mol.%. All had typical interconnected cellular morphology, which was not affected by the hypercrosslinking process. Nitrogen adsorption and desorption experiments with BET and t-plot modelling were used for the evaluation of the newly introduced nanoporosity and in combination with elemental analysis for the evaluation of the extent of the hypercrosslinking. It was found that, for all three initial crosslinking degrees, the minimum amount of functional monomer, 4-vinylbenzyl chloride, was approximately 30 mol.%. Hypercrosslinking of polymers with lower concentrations of functional monomer did not result in induction of nanoporosity while the initial crosslinking degree had a much lower impact on the formation of nanoporosity.

16.
Plants (Basel) ; 10(4)2021 Mar 30.
Artigo em Inglês | MEDLINE | ID: mdl-33808171

RESUMO

In view of growing requirements of the food industry regarding elderberries (genus Sambucus), a need to increase their productivity and improve their chemical composition has emerged. With this purpose in mind, numerous elderberry interspecific hybrids have been created. In the present work, the content of minerals in their crucial plant parts was studied. It was also investigated whether superior genotypes regarding the mineral composition of berries and inflorescences could be predicted at early stages of plant development. The results showed that elderberry leaves contained the highest amounts of Ca, Mg, Mn, Zn, and Sr, while K and P were predominant in fruit stalks. Fe and Al prevailed in roots and Cu in bark. Although berries showed lower mineral content compared to other plant parts, their mineral content is not negligible and could be comparable to other commonly consumed berries. Genotypes with a favorable mineral content of inflorescences and berries could be predicted on the basis of known mineral composition of their shoots and leaves. The study also indicates that S. nigra genotypes and the majority of interspecific hybrids analyzed are suitable for further genetic breeding or cultivation.

17.
Sensors (Basel) ; 21(9)2021 Apr 23.
Artigo em Inglês | MEDLINE | ID: mdl-33922519

RESUMO

A novel promising carbon paste electrode with excellent potentiometric properties was prepared for the analysis of trihexyphenidyl hydrochloride (THP), the acetylcholine receptor and an anticholinergic drug in real samples. It contains 10.2% trihexyphenidy-tetraphenylborate ionic pair as the electroactive material, with the addition of 3.9% reduced graphene oxide and 0.3% of anionic additive into the paste, which consists of 45.0% dibutylphthalate as the solvent mediator and 40.6% graphite. Under the optimized experimental conditions, the electrode showed a Nernstian slope of 58.9 ± 0.2 mV/decade with a regression coefficient of 0.9992. It exhibited high selectivity and reproducibility as well as a fast and linear dynamic response range from 4.0 × 10-7 to 1.0 × 10-2 M. The electrode remained usable for up to 19 days. Analytical applications showed excellent recoveries ranging from 96.8 to 101.7%, LOD was 2.5 × 10-7 M. The electrode was successfully used for THP analysis of pharmaceutical and biological samples.


Assuntos
Grafite , Preparações Farmacêuticas , Carbono , Eletrodos , Potenciometria , Reprodutibilidade dos Testes , Triexifenidil
18.
Molecules ; 26(9)2021 Apr 23.
Artigo em Inglês | MEDLINE | ID: mdl-33922767

RESUMO

When dealing with simple phenols such as caffeic acid (CA) and ferulic acid (FA), found in a variety of plants, it is very important to have control over the most important factors that accelerate their degradation reactions. This is the first report in which the stabilities of these two compounds have been systematically tested by exposure to various different factors. Forced degradation studies were performed on pure standards (trans-CA and trans-FA), dissolved in different solvents and exposed to different oxidative, photolytic and thermal stress conditions. Additionally, a rapid, sensitive, and selective stability-indicating gas chromatographic-mass spectrometric method was developed and validated for determination of trans-CA and trans-FA in the presence of their degradation products. Cis-CA and cis-FA were confirmed as the only degradation products in all the experiments performed. All the compounds were perfectly separated by gas chromatography (GC) and identified using mass spectrometry (MS), a method that additionally elucidated their structures. In general, more protic solvents, higher temperatures, UV radiation and longer storage times led to more significant degradation (isomerization) of both trans-isomers. The most progressive isomerization of both compounds (up to 43%) was observed when the polar solutions were exposed to daylight at room temperature for 1 month. The method was validated for linearity, precision as repeatability, limit of detection (LOD) and limit of quantitation (LOQ). The method was confirmed as linear over tested concentration ranges from 1-100 mg L-1 (r2s were above 0.999). The LOD and LOQ for trans-FA were 0.15 mg L-1 and 0.50 mg L-1, respectively. The LOD and LOQ for trans-CA were 0.23 mg L-1 and 0.77 mg L-1, respectively.


Assuntos
Ácidos Cafeicos/química , Ácidos Cumáricos/química , Cromatografia Gasosa-Espectrometria de Massas/métodos , Cromatografia Líquida de Alta Pressão
19.
Molecules ; 25(21)2020 Nov 09.
Artigo em Inglês | MEDLINE | ID: mdl-33182383

RESUMO

A new modified ion-selective electrode with membranes of LaF3 single crystals with different internal contacts (solid steel or electrolyte) and with FexOy nanoparticles as loading was developed. The best response characteristic with linear potential change was found in the fluoride concentration range from 10-1 to 3.98 × 10-7 M. The detection limit for the electrolyte contact was determined at 7.41 × 10-8 M with a regression coefficient of 0.9932, while the regression coefficient for the solid contact was 0.9969. The potential change per concentration decade ranged from 50.3 to 62.4 mV, depending on whether the contact was solid or electrolytic. The prepared modified electrode has a long lifetime, as well as the possibility of application in different positions (solid contact), and it can also be used for the determination of iron ions. The electrode characterization was performed with scanning electron microscopy and elemental analysis with the technique of electron-dispersive X-ray spectroscopy.


Assuntos
Eletrodos , Fluoretos/química , Íons , Nanopartículas Metálicas/química , Nanotecnologia/métodos , Concentração de Íons de Hidrogênio , Lantânio/química , Limite de Detecção , Modelos Lineares , Metais/química , Microscopia Eletrônica de Varredura , Espectroscopia Fotoeletrônica , Potenciometria/métodos
20.
Front Chem ; 8: 582746, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-33173770

RESUMO

The formation of metal complexes with phytic acid is a complex process that depends strongly on the metal-to-ligand molar ratio, pH value and consequent protonation level of the phytate ligand as well as accompanying side reactions, in particular metal hydrolysis and precipitation of the formed coordination compounds. In the present work, the potentiometric titration technique was used in combination with a detailed analysis of the equivalent point dependencies for selected biologically relevant monovalent and divalent cations from the groups of alkaline earths and transition metals, namely: Mg(II), Zn(II), Fe(II), Cu(I), and Cu(II) ions. The investigation of complex formation mechanism, the evaluation of the species formed, and the identification of other side reactions was based on the examination of three distinct equivalent points, which were detectable by alkalimetric titrations of phytic acid in the presence of selected metal ions. It has been demonstrated that alkaline earth metals interact with different binding site(s) than the transition metals, and experiments with both oxidation states of copper revealed similar complexing characteristics, which depend mainly on the ionic radius (and not on the ionic charge as initially expected). Quantitative data on phytate complexation, hydroxide formation and complex precipitation are presented herein for all metals studied, including Cu(I), which was investigated for the first time by means of alkalimetric titration.

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