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1.
Int J Mol Sci ; 25(6)2024 Mar 09.
Artigo em Inglês | MEDLINE | ID: mdl-38542141

RESUMO

Claudin polymers constitute the tight junction (TJ) backbone that forms paracellular barriers, at least for bigger solutes. While some claudins also seal the barrier for small electrolytes, others form ion channels. For cation-selective claudin-15 and claudin-10b, structural models of channels embedded in homo-polymeric strands have been suggested. Here, we generated a model for the prototypic anion-selective claudin-10a channel. Based on previously established claudin-10b models, dodecamer homology models of claudin-10a embedded in two membranes were analyzed by molecular dynamics simulations. The results indicate that both claudin-10 isoforms share the same strand and channel architecture: Sidewise unsealed tetrameric pore scaffolds are interlocked with adjacent pores via the ß1ß2 loop of extracellular segment 1. This leads to TJ-like strands with claudin subunits arranged in four joined rows in two opposing membranes. Several but not all cis- and trans-interaction modes are indicated to be conserved among claudin-10a, -10b, and -15. However, pore-lining residues that differ between claudin-10a and -10b (i.e., R33/I35, A34/D36, K69/A71, N54/D56, H60/N62, R62/K64) result in opposite charge selectivity of channels. This was supported by electric field simulations for both claudins and is consistent with previous electrophysiological studies. In summary, for the first time, a structural and mechanistic model of complete and prototypic paracellular anion channels is provided. This improves understanding of epithelial paracellular transport.


Assuntos
Claudinas , Simulação de Dinâmica Molecular , Claudinas/metabolismo , Canais Iônicos , Junções Íntimas/metabolismo , Ânions/análise
2.
J Chromatogr A ; 1720: 464769, 2024 Apr 12.
Artigo em Inglês | MEDLINE | ID: mdl-38442499

RESUMO

In this study, we introduce a novel approach for the analysis of salivary ions using capillary electrophoresis (CE) with a triple-layer coated capillary. The capillary is sequentially coated with cationic silylating reagents, poly(vinylsulfonate), and polybrene to form a custom designed surface that effectively inhibits adsorption of protein matrix on the capillary inner wall and allows for reproducible ion analysis. For the CE with capacitively coupled contactless conductivity detection, we used suitable background electrolytes (BGEs) for salivary ion analysis. Anions were separated using a mixture of 2-(N-morpholino)ethanesulfonic acid and l-arginine, and cations were separated using that with 18-crown-6. This setup enabled rapid separation, within 4 min, together with sensitive detection. We quantified nine common anions and five cations typically found in saliva samples using this CE method, both before and after a cold pressure test (CPT, a standard stress test). The CE system demonstrated consistent ion separation across 30 consecutive measurements without requiring capillary replacement. Notably, the salivary ion balance remained predominantly anion-rich, regardless of the CPT. Cold water exposure induced greater variation in the total anion concentration than in the total cation concentration. Further analysis using multiple regression analysis revealed strong relationships between nitrate and nitrite, formate and phosphate, and potassium and nitrate, before and after the CPT. Notably, potassium and nitrate ions exhibited variations in response to stress. These results provided a method for assessing salivary ion composition and insights into the potential of salivary ions as biomarkers for stress.


Assuntos
Eletroforese Capilar , Nitratos , Cátions/análise , Ânions/análise , Eletroforese Capilar/métodos , Água , Potássio
3.
Cornea ; 43(2): 172-177, 2024 Feb 01.
Artigo em Inglês | MEDLINE | ID: mdl-37404128

RESUMO

PURPOSE: Tear fluid (TF) contains a variety of electrolytes that exhibit a strong correlation with its osmotic pressure. These electrolytes are also related to the etiology of diseases on ocular surfaces such as dry eye syndromes and keratopathy. Although positive ions (cations) in TF have been investigated to understand their roles, negative ions (anions) have hardly been studied because applicable analytical methods are restricted to a few kinds. In this study, we established a method to analyze the anions involved in a sufficiently small amount of TF for in situ diagnosis of a single subject. METHODS: Twenty healthy volunteers (10 men and 10 women) were recruited. Anions in their TF were measured on a commercial ion chromatograph (IC-2010, Tosoh, Japan). Tear fluid (5 µL or more) was collected from each subject with a glass capillary, diluted with 300 µL of pure water, and conveyed to the chromatograph. We successfully monitored the concentrations of bromide, nitrate, phosphate, and sulfate anions (Br - , NO 3- , HPO 42- , and SO 42- , respectively) in TF. RESULTS: Br - and SO 42- were universally detected in all samples, whereas NO 3- was found in 35.0% and HPO 42- in 30.0% of them. The mean concentrations (mg/L) of each anion were Br - , 4.69 ± 0.96; NO 3- , 0.80 ± 0.68; HPO 42- , 17.48 ± 7.60; and SO 42- , 3.34 ± 2.54. As for SO 42- , no sex differences or diurnal variations were observed. CONCLUSIONS: We established an efficient protocol to quantitate various inorganic anions involved in a small amount of TF using a commercially available instrument. This is the first step to elucidate the role of anions in TF.


Assuntos
Cromatografia , Água , Masculino , Feminino , Humanos , Ânions/análise , Eletrólitos/química , Nitratos
4.
J Environ Sci (China) ; 138: 496-505, 2024 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-38135415

RESUMO

Zhuzhou was one of the most polluted cities in China with the serious acid rain. Due to the implementation of air pollution control measures from 2016 to 2018, the acid rain pollution in this city has reduced. In order to understand the recent situation, a comprehensive study on the acid rain was carried out from January 2011 to December 2020. The pH values during the study period varied from 3.3 to 7.5, with a volume-weighted mean value of 4.7. The predominant acidic components of the precipitation were SO42- and NO3-, accounting for 89.3% of the total anions. The ratio of non-sea-salt SO42- to NO3- showed a decreasing trend, revealing that the pollution type of acid rain changed from sulfuric acid type to sulfuric acid and nitric acid compound type. The correlation analysis (p < 0.05) showed that SO42- was positively correlated with NH4+, Ca2+, and Mg2+; hence, it predominated in precipitation as (NH4)2SO4, NH4HSO4, CaSO4, and MgSO4. Significant positive correlation of Ca2+ with Mg2+ shows that they may originated mainly from crust. Significant positive correlation between SO42- and F- and Cl- indicate that their source may be related to the non-ferrous metal smelting industry in Zhuzhou. Further correlation analysis shows that emissions from the non-ferrous metal smelting industry in the area have a large significant on SO42- and F- in precipitation, while Cl- may still be emitted from other anthropogenic sources.


Assuntos
Chuva Ácida , Poluentes Atmosféricos , Chuva Ácida/análise , Monitoramento Ambiental , Ânions/análise , China , Estações do Ano , Poluentes Atmosféricos/análise
5.
J Chromatogr A ; 1711: 464464, 2023 Nov 22.
Artigo em Inglês | MEDLINE | ID: mdl-37871504

RESUMO

We report a battery powered non-suppressed open tubular ion chromatograph (NSOTIC) that weighs less than 3 kg with on-board rechargeable lithium-ion batteries that provide power for 18 h of operation. It is contained in an aluminum case measuring 30 × 25 × 16 cm. Separation relies on open tubular (OT) chromatographic columns which eliminate the need for high pressure pumps, drastically reducing weight and complexity. Eluent consumption is less than 100 µL per separation. Eluent is supplied from a pressurized vessel via a voltage-controlled electronic pressure controller. Flow rates are typically <200 nL/min which allows a single 16-20 g gas cartridge to perform hundreds of separations. Two anions, chloride and nitrate, in Atacama soil samples were field determined by running the portable NSOTIC. More samples were lab analyzed by commercial IC and IC/MS-MS (only perchlorate due to its low concentration level). To demonstrate the feasibility of running NSOTIC on sample analysis, samples were tested by both non-portable and portable NSOTIC.


Assuntos
Cromatografia , Nitratos , Ânions/análise , Compostos Orgânicos , Cloretos , Cromatografia por Troca Iônica
6.
ACS Sens ; 8(8): 3225-3239, 2023 08 25.
Artigo em Inglês | MEDLINE | ID: mdl-37530141

RESUMO

We report here a small library of a new type of acyclic squaramide receptors (L1-L5) as selective ionophores for the detection of ketoprofen and naproxen anions (KF- and NS-, respectively) in aqueous media. 1H NMR binding studies show a high affinity of these squaramide receptors toward KF- and NS-, suggesting the formation of H-bonds between the two guests and the receptors through indole and -NH groups. Compounds L1-L5 have been tested as ionophores for the detection of KF- and NS- inside solvent PVC-based polymeric membranes. The optimal membrane compositions were established through the careful variation of the ligand/tridodecylmethylammonium chloride (TDMACl) anion-exchanger ratio. All of the tested acyclic squaramide receptors L1-L5 have high affinity toward KF- and NS- and anti-Hofmeister selectivity, with L4 and L5 showing the highest sensitivity and selectivity to NS-. The utility of the developed sensors for a high precision detection of KF- in pharmaceutical compositions with low relative errors of analysis (RSD, 0.99-1.4%) and recoveries, R%, in the range 95.1-111.8% has been demonstrated. Additionally, the chemometric approach has been involved to effectively discriminate between the structurally very similar KF- and NS-, and the possibility of detecting these analytes at concentrations as low as 0.07 µM with R2 of 0.947 and at 0.15 µM with R2 of 0.919 for NS- and KF-, respectively, was shown.


Assuntos
Quinina , Ionóforos/química , Ânions/análise
7.
Water Res ; 243: 120324, 2023 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-37451124

RESUMO

Anion exchange resin (AER) and granular activated carbon (GAC) have emerged as prominent technologies for treatment of waters contaminated with per- and polyfluoroalkyl substances (PFASs). This study compares the life cycle environmental impacts and life cycle costs of remediating PFAS-contaminated groundwater with these competing technologies, using field pilot data to inform model inputs. Comparative analysis indicates that AER systems employing single-use "PFAS-selective" resins have lower environmental impacts and costs than systems using regenerable resins or GAC adsorbents, supporting its use in future remediation efforts. Use of GAC operated as a single-use adsorbent led to the highest emissions as well as the highest treatment costs, with thermally-reactivated GAC proving to be less impactful than regenerable AER treatment. Sensitivity analyses highlighted the dominance of media usage rate (MUR), which is highly dependent on the selected PFAS treatment goals, to determine environmental impacts and costs over a 30-year system life cycle. Selection of very stringent changeout criteria (e.g., detection of any PFASs in effluent) significantly reduces the advantages of single-use resins. For regenerable AER, environmental impacts were dominated by management of the PFAS-contaminated brine/co-solvent waste stream used to regenerate the adsorbent, as well as the cosolvent content of the regenerant mixture and the cosolvent recovery efficiency achieved via on-site distillation. High impacts estimated for GAC adsorption, the result of high MUR relative to ion exchange media, can be significantly reduced if spent adsorbents are reused after thermal reactivation, but impacts are still greater than those predicted for single-use ion exchange systems. Findings are expected to hold across a range of diverse sites, including drinking water systems treating more dilute sources of PFAS contamination, as PFAS breakthrough was not found to be highly sensitive to sourcewater PFAS concentrations.


Assuntos
Fluorocarbonos , Água Subterrânea , Poluentes Químicos da Água , Animais , Carvão Vegetal , Fluorocarbonos/análise , Poluentes Químicos da Água/análise , Ânions/análise , Resinas de Troca Aniônica , Custos e Análise de Custo , Estágios do Ciclo de Vida
8.
Environ Monit Assess ; 195(6): 653, 2023 May 10.
Artigo em Inglês | MEDLINE | ID: mdl-37162599

RESUMO

This study characterises the quality of groundwater for the Ludhiana district of Punjab, India by analysing water samples collected from 152 locations spread across 3767 km2. The samples were analysed for 18 parameters consisting of pH, EC, TDS, TA, TH, major anions and cations. The parameter values have been used to calculate the drinking water quality index of the study area which suggests that 2.6, 57.9, 32.9, 4 and 2.6% of the samples fall under the excellent, good, poor, very poor and unsuitable categories, respectively. The sequence of abundance for ions (in meq/l) as revealed from the laboratory tests is Na+ (37.1%) > Ca2+ (30.8%) > Mg2+ (29.1%) > K+ (2.8%) for cations and HCO3- (80%) > Cl¯ (8.9%) > CO32- (6.5%) > SO42- (3.9%) > NO3-, F-, PO43- (< 1%) for anions. The spatial variability of these parameters has been depicted through the use of interpolation maps. Evaluation of different ionic ratios indicates that carbonate weathering and silicate weathering are both significantly affecting the groundwater chemistry with a slight dominance of carbonate weathering. Also, the ion exchange process is taking place in the area as confirmed by CAI index values. In terms of saturation index, the groundwater is undersaturated with respect to halite, fluorite and sylvite, whereas it is supersaturated for calcite, dolomite and aragonite minerals. The principal components in PCA explained 75.4% of the total variance with 29.1 and 28.3% contributions from PC1 and PC2. Both of these components indicate towards the geogenic and anthropogenic influence on groundwater mineralization of the area. The analysis suggests that groundwater for the study area is suitable for drinking in most of the region expect in a few places. Such a study could be used to understand the current status of groundwater quality in the area, the results of which can be used to prevent further contamination and sustain the resource for the future.


Assuntos
Água Potável , Água Subterrânea , Poluentes Químicos da Água , Água Potável/análise , Monitoramento Ambiental/métodos , Poluentes Químicos da Água/análise , Qualidade da Água , Água Subterrânea/análise , Ânions/análise , Carbonatos/análise , Cátions/análise , Índia
9.
J Chromatogr A ; 1694: 463908, 2023 Apr 12.
Artigo em Inglês | MEDLINE | ID: mdl-36913814

RESUMO

Ion chromatography (IC) has grown in usage rapidly since its first introduction in 1975. However, IC is still sometimes unable to separate target analytes from coexisting components well with identical elution time, due to the limited resolution and column capacity, especially in the presence of high-level salt matrix. These limitations hence drive IC to develop two-dimensional IC (2D-IC). In this review, we capture the 2D-IC applications in environmental samples via the perspective of coupling different IC columns, which aim to summarize where these 2D-IC methods fit in. In sequence, we firstly review the principles of 2D-IC and emphasize one-pump column-switching IC (OPCS IC) because it is a simplified 2D-IC that only uses one set of IC system. We then compare typical 2D-IC and OPCS IC performances in terms of application scope, method detection limit, drawbacks, and expectations. Finally, we propose some challenges of current methods and opportunities for future research. For instance, it is challenging to couple anion exchange column and capillary column in OPCS IC due to the incompatibility between flow path dimensions and suppressor; coupling ion exclusion column and mixed-bed column may be promising to simultaneously determine anions and cations in weak acids or salts. The details of this study may help practitioners to better understand and implement 2D-IC methods and meanwhile motivate researchers to fill in the knowledge gap in the future.


Assuntos
Ácidos , Cromatografia por Troca Iônica/métodos , Ânions/análise , Ácidos/química , Cátions
10.
Environ Sci Pollut Res Int ; 30(49): 107138-107157, 2023 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-36892700

RESUMO

This research was conducted in the urban area of Patna region, the capital and largest city of Bihar, which is part of the Indo-Gangetic alluvium plain. This study aims to identify the sources and processes controlling groundwater's hydrochemical evolution in the Patna region's urban area. In this research, we evaluated the interplay between several measures of groundwater quality, the various possible causes of groundwater pollution, and the resulting health risks. Twenty groundwater samples were taken from various locations and examined to determine the water quality. The average EC of the groundwater in the investigated area was 728 ± 331.84 µS/cm, with a range of around 300-1700 µS/cm. Positive loadings were seen for total dissolved solids (TDS), electrical conductivity (EC), calcium (Ca2+), magnesium (Mg2+), sodium (Na+), chloride (Cl-), and sulphate (SO42-) in principal component analysis (PCA), demonstrating that these variables accounted for 61.78% of the total variance. In the groundwater samples, the following main cations are the most prevalent such as Na+ > Ca2+ > Mg2+ > K+, while the dominant anions are HCO3- > Cl- > SO42-. The elevated HCO3- and Na+ ions indicate that carbonate mineral dissolution might affect the study area. The result demonstrated that 90% of samples fall into the Ca-Na-HCO3 type, remaining in the mixing zone. The presence of the NaHCO3 kind of water is suggestive of shallow meteoric water, which may have originated from the river Ganga that is located nearby. The results show that a multivariate statistical analysis and graphical plots successfully identify the parameters controlling groundwater quality. In accordance with guidelines for safe drinking water, the electrical conductivity and potassium ion concentrations in the groundwater samples are 5% higher than acceptable levels. People who take large amounts of salt replacements report feeling tight in the chest, vomiting, having diarrhoea, developing hyperkalaemia, having trouble breathing, and even experiencing heart failure.


Assuntos
Água Subterrânea , Poluentes Químicos da Água , Humanos , Monitoramento Ambiental , Poluentes Químicos da Água/análise , Qualidade da Água , Água Subterrânea/análise , Ânions/análise , Cloretos/análise , Sódio/análise
11.
Environ Monit Assess ; 195(2): 316, 2023 Jan 21.
Artigo em Inglês | MEDLINE | ID: mdl-36670262

RESUMO

The present study has been carried out to assess the quality of groundwater and surface water resources of Thettiyar watershed, Kerala, India. Sixty-six water samples were collected during pre-monsoon (April, 2019) and monsoon (July, 2019) season, and analyzed for pH, electrical conductivity (EC), total dissolved solids (TDS), total hardness and major cations and anions and microbiological parameters as well. According to the piper diagram's plot, Ca and Mg dominate over Na among the cations, and Cl is the most prevalent anion in groundwater throughout both the studied seasons. The hydrochemical analysis of water samples revealed that all the parameters are within the permissible limit except for pH. For microbiological analysis, the samples were tested for total coliform and fecal coliform. Most of the groundwater samples collected have higher total coliform and fecal coliform (E. coli) content than the recommended count by BIS (2012). The pre-monsoon surface water samples owned a maximum number of 3700 cfu/100 ml (TNTC-too numerous to count) of total coliform and 1400 cfu/100 ml (TNTC) of fecal coliform. In monsoon, the number of total coliform and fecal coliform has increased to 3800 cfu/100 ml and 1900 cfu/100 ml respectively. E. coli and total coliform are effectively correlated with each other in both seasons, in accordance with the statistical study. Domestic, sewage dump, and other household wastes are the main sources of bacterial contamination in the study area, which in turn nourishes contaminant organisms. According to the results, the government or municipality should implement an appropriate system for managing solid waste and should take all necessary measures to clean up the study area.


Assuntos
Água Subterrânea , Poluentes Químicos da Água , Qualidade da Água , Monitoramento Ambiental/métodos , Sistemas de Informação Geográfica , Escherichia coli , Poluentes Químicos da Água/análise , Água Subterrânea/química , Ânions/análise , Água/análise , Cátions/análise , Índia
12.
Anal Methods ; 15(3): 311-321, 2023 01 19.
Artigo em Inglês | MEDLINE | ID: mdl-36562458

RESUMO

Shrimp is one of the most traded fishery products in the world. The shrimp-farming water ionic composition is fundamental to the growth and survival of these specimens. Therefore, this study is aimed to develop a method for the simultaneous separation of Cl-, SO42-, NO3-, NO2-, and HCO3- in this sample by capillary zone electrophoresis with UV indirect detection, without any prior sample treatment, besides dilution. The background electrolyte (BGE) was composed of CrO42- (60 mmol L-1), cetyltrimethylammonium bromide (CTAB, 2.5 mmol L-1), acetonitrile (0.875% (v/v)), and methanol (2.625% (v/v)). The mixture design optimized the BGE composition. Acetonitrile and methanol changed the degree of solvation of the anions, which decreased the radius, a phenomenon proven by calculating the radius of anions in all the conditions of the mixture design. The optimized and validated method allowed the simultaneous determination of the five above-mentioned anions in 10 min.


Assuntos
Dióxido de Nitrogênio , Água , Metanol , Eletrólitos , Ânions/análise , Agricultura
13.
Inorg Chem ; 62(1): 56-65, 2023 Jan 09.
Artigo em Inglês | MEDLINE | ID: mdl-36576501

RESUMO

A series of two-dimensional (2D) polyoxometalate-based frameworks, [Ln3(PDA)3(H2O)6(PMo12O40)]·xH2O (Ln = La (1); Ce (2); Pr (3); Nd (4); PDA = 1,10-phenanthroline-2,9-dicarboxylate), have been synthesized and structurally characterized by various analytical techniques. Single-crystal X-ray diffraction reveals that 1-4 have a unique 2D layer structure in which Keggin anions have coordinated upward and downward the plane, and this feature makes them suitable candidates for surface binding of common drugs via supramolecular and electrostatic interactions. Also, the ability of 1-4 (as the first polyoxomolybdate-containing frameworks) as sorbents for the extraction and quantitative determination of opioid drugs (morphine, methadone, and pethidine) was investigated by using dispersive micro-solid-phase extraction (D-µSPE) and high-performance liquid chromatography (HPLC). The method showed wide linear ranges in the range of 0.3 to 300 ng mg-1 and low limits of detection (LODs) ranged from 0.1 to 0.2 ng mg-1 of hair.


Assuntos
Analgésicos Opioides , Cabelo , Analgésicos Opioides/análise , Ânions/análise , Limite de Detecção , Cromatografia Líquida de Alta Pressão/métodos , Cabelo/química
14.
Environ Sci Pollut Res Int ; 30(11): 29407-29431, 2023 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-36414896

RESUMO

The quality of groundwater in the Jaunpur district of Uttar Pradesh is poorly studied despite the fact that it is the only supply of water for both drinking and irrigation and people use it without any pre-treatment. The evaluation of groundwater quality and suitability for drinking and irrigation is presented in this study. Groundwater samples were collected and analysed by standard neutralisation and atomic emission spectrophotometry for major anions (HCO3-, SO42-, Cl-, F-, NO3-), cations (Ca2+, Mg2+, Na+, K+), and heavy metals (Cd, Mn, Zn, Cu, and Pb). The geographic information system (GIS) and statistical inferences were utilised for the spatial mapping of the groundwater's parameters. The potential water abstraction (i.e. taking water from sources such as rivers, streams, canals, and underground) for irrigation was assessed using the sodium absorption ratio (SAR), permeability index (PI), residual sodium carbonate (RSC), and Na percentage. According to the findings, the majority of the samples had higher EC, TDS, and TH levels, indicating that they should be avoided for drinking and irrigation. The positive correlation coefficient between chemical variability shows that the water chemistry of the studied region is influenced by geochemical and biological causes. According to the USSL (United States Salinity Laboratory) diagram, most of the samples fall under the C2-S1 and C3-S1 moderate to high salt categories. Some groundwater samples were classified as C4-S3 class which is unfit for irrigation and drinking. This study suggests that the groundwater in the study area is unfit for drinking without treatment. However, the majority of the samples were suitable for irrigation.


Assuntos
Água Potável , Água Subterrânea , Poluentes Químicos da Água , Humanos , Sistemas de Informação Geográfica , Monitoramento Ambiental , Água Subterrânea/análise , Ânions/análise , Sódio/análise , Água/análise , Qualidade da Água , Poluentes Químicos da Água/análise , Água Potável/análise , Índia
15.
Appl Radiat Isot ; 192: 110566, 2023 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-36493679

RESUMO

89SrCl2 radiopharmaceuticals is mainly used for bone pain palliation in the cancer patients, is being produced in FBTR via 89Y(n, p)89Sr using yttria target. The irradiated yttria target is chemically processed in high pure quartz distilled nitric acid medium in hot cell facility, to avoid the corrosion of components of hotcell due to chloride ions while using HCl medium. Being ionic species, the purified 89Sr(II) cation in aqueous solution containing bulk nitrate and other trace anions, exists as SrXn species where X: F-, Cl-, Br-, NO3-, PO43- and SO42-, n: stoichiometric anion content. The aim of the manuscript is to standardise an efficient ultra-low level anion purification method (ppb range) for the conversion of SrXn to SrCl2 and estimate the residual anionic impurities as recommended by the appropriate source specifications for its medical application. Various methods were standardised for the removal of anions in the SrCl2 source produced by the above process which include evaporation, calcination, anion exchange column, cation exchange column as well as its combination with pre-concentration column of ion chromatography (IC) technique using 89Sr tracers as well as FBTR produced 89Sr solution. Assay of 89Sr and other anions including nitrate for the above study were accomplished using Cerenkov counting and ion chromatography respectively. Thus evaporation-calcination-column chromatography mode was finalised to obtain pure SrCl2 source free from nitrate and other anionic impurities. This is the first ever systematic study for the Radiochemical quality control of nca 89SrCl2 radiopharmaceutical produced in a fast reactor. This study also finds its application to any analytical lab as well as industry where there is a requirement of anion purification in the ppb level.


Assuntos
Nitratos , Compostos Radiofarmacêuticos , Humanos , Nitratos/análise , Nitratos/química , Cromatografia por Troca Iônica/métodos , Ânions/análise , Cátions/análise , Controle de Qualidade
16.
Anal Bioanal Chem ; 415(5): 759-774, 2023 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-36472636

RESUMO

Isotope ratios of methylmercury (MeHg) within organisms can be used to identify sources of MeHg that have accumulated in food webs, but these isotopic compositions are masked in organisms at lower trophic levels by the presence of inorganic mercury (iHg). To facilitate measurement of MeHg isotope ratios in organisms, we developed a method of extracting and isolating MeHg from fish and aquatic invertebrates for compound-specific isotopic analysis involving nitric acid digestion, batch anion-exchange resin separation, and pre-concentration by purge and trap. Recovery of MeHg was quantified after each step in the procedure, and the average cumulative recovery of MeHg was 93.4 ± 2.9% (1 SD, n = 28) for biological reference materials and natural biota samples and 96.9 ± 1.8% (1 SD, n = 5) for aqueous MeHgCl standards. The amount of iHg impurities was also quantified after each step, and the average MeHg purity was 97.8 ± 4.3% (1 SD, n = 28) across all reference materials and natural biota samples after the final separation step. Measured MeHg isotopic compositions of reference materials agreed with literature values obtained using other MeHg separation techniques, and MeHg isotope ratios of aqueous standards, reference materials, and natural biota samples were reproducible. On average, the reproducibility associated with reference material process replicates (2 SD) was 0.10‰ for δ202MeHg and 0.04‰ for Δ199MeHg. This new method provides a streamlined, reliable technique that utilizes a single sample aliquot for MeHg concentration and isotopic analysis. This promotes a tight coupling between MeHg concentration, %MeHg, and Hg isotopic composition, which may be especially beneficial for studying complex food webs with multiple isotopically distinct sources of iHg and/or MeHg.


Assuntos
Mercúrio , Compostos de Metilmercúrio , Poluentes Químicos da Água , Animais , Compostos de Metilmercúrio/análise , Ácido Nítrico/análise , Isótopos de Mercúrio/análise , Reprodutibilidade dos Testes , Monitoramento Ambiental/métodos , Poluentes Químicos da Água/análise , Mercúrio/análise , Cadeia Alimentar , Isótopos/análise , Digestão , Ânions/análise
17.
AAPS J ; 25(1): 3, 2022 11 22.
Artigo em Inglês | MEDLINE | ID: mdl-36414847

RESUMO

The genome content of adeno-associated virus (AAV) vectors is critical to the safety and potency of AAV-based gene therapy products. Empty capsids are considered a product-related impurity and a critical quality attribute (CQA) of the drug product, thus requiring characterization throughout the production process to demonstrate they are controlled to acceptable levels in the final drug product. Anion exchange chromatography has been used to achieve separation between empty and full capsids, but requires method development and gradient optimization for different serotypes and formulations. Here, we describe an alternative approach to quantitation that does not rely on achieving separation between empty and full capsids, but instead uses the well-established relationship between absorbance at UV A260/A280 and relation to DNA/protein content, in combination with anion-exchange chromatography to allow one to calculate the relative proportion of empty and full capsids in AAV samples from a single peak. We call this approach ACUVRA: Anion-exchange Chromatography UV-Ratio Analysis, and show the applicability of the method through a case study with recombinant AAV2 (rAAV2) process intermediates and drug substance. Method qualification and GMP validation in a quality control (QC) laboratory results show that ACUVRA is a fit-for-purpose method for process development support and characterization, while also being a QC-friendly option for GMP release testing at all stages of clinical development. Graphical abstract.


Assuntos
Capsídeo , Dependovirus , Dependovirus/genética , Capsídeo/química , Vetores Genéticos , Cromatografia , Ânions/análise , Controle de Qualidade
18.
Anal Chem ; 94(45): 15546-15552, 2022 11 15.
Artigo em Inglês | MEDLINE | ID: mdl-36342126

RESUMO

A new analytical methodology, using capillary electrophoresis in indirect UV absorbance mode, is developed for the quantification of analytes in the absence of reference materials. The methodology allows the quantification of organic molecules and/or small ions, anionic or cationic, absorbing or not in the UV range, carrying either one or two electric charges. Two methods of data processing were compared. The first is based on the use of a dynamic simulator of electromigration, and the second uses the Kohlrausch regulating function combined with the electroneutrality equation. The experimental conditions presented in this work allow a precise quantification of anions having electrophoretic mobilities (µep) between -22.71 and -36.92 × 10-9 m2 V-1 s-1 and cations with µep between +30.59 and +63.60 × 10-9 m2 V-1 s-1 with percent relative errors lower than -5.52%. The effect of the integration errors on the reliability of the results is discussed in detail.


Assuntos
Eletricidade , Eletroforese Capilar , Reprodutibilidade dos Testes , Ânions/análise , Cátions , Eletroforese Capilar/métodos
19.
Environ Monit Assess ; 195(1): 29, 2022 Oct 25.
Artigo em Inglês | MEDLINE | ID: mdl-36282453

RESUMO

The aim of the study was to determine the groundwater characteristics of rural and industrial zones in the Kannur region. In 2011, 25 groundwater data were collected from the centre for water resource development management (CWRDM), and in 2019, 25 groundwater samples from rural and near-industrial areas were collected and analysed for major anions (HCO3-, CO32-, Cl-, NO3- and SO42-), and cations (TH, Ca2+, Mg2+, Na+, K+ and Fe2+) using APHA standards. To better understand the link between water quality parameters, multivariate statistical analysis approaches such as principal component analysis (PCA), hierarchical cluster analysis (HCA), correlation matrix analysis (CMA), and Pearson correlation bivariate one-tailed analysis (PCBOTA) were used to analyse the inter-relationship of data. The Inverse Distance Weighed (IDW) method was used to generate the spatial distribution of the groundwater quality index (GWQI). In 2011, the water quality index (WQI) value of groundwater samples was excellent at 24.42% and good at 54.14%, which were used for drinking purposes and moderate at 17.22% and poor at 4.22% for irrigation purposes in this study area. In 2019, excellent 21.62%, good 51.56% were used for drinking purpose, and moderate at 18.14%, and poor at 8.68% for irrigation purposes. By comparing the data with BIS and WHO standards, it is clear that groundwater in Kannur district is of good quality. In groundwater samples, the PCA eigen values were reported in 2011 (84.7%) and 2019 (73.4%) for statistical approaches. This study uses HCA and PCBOTA to analyse the elements, resulting in a better understanding of groundwater quality development. GIS based WQI maps were obtained and utilised to gain a better knowledge of the study area's past and present water quality status. We observed that the quality of groundwater in the study region's north-western portion is insufficient for drinking water.


Assuntos
Água Potável , Água Subterrânea , Poluentes Químicos da Água , Sistemas de Informação Geográfica , Água Potável/análise , Monitoramento Ambiental/métodos , Poluentes Químicos da Água/análise , Água Subterrânea/análise , Qualidade da Água , Ânions/análise , Cátions/análise , Índia
20.
Environ Monit Assess ; 194(12): 920, 2022 Oct 18.
Artigo em Inglês | MEDLINE | ID: mdl-36257995

RESUMO

The present study quantified element concentrations and evaluated the removal efficiencies of the Lufkin Wastewater Treatment Plant (LWWTP): a public municipal wastewater treatment plant in East Texas. Macroelements (Na, K, Mg, Ca, Al, Fe, Se, Zn, P, and S) and microelements (Ni, Pb, Mn, Cr, Mo, Cu, Co, V, As, B, Ba) were detected using ICP-OES and ICP-MS. In addition, the anion concentrations (Br-, NO3-, NO2-, PO43-, F-, Cl-, and SO42-) and their percent removal from the LWWTP were assessed by using ion chromatography. Whereas macroelements in the influent were above the maximum ceiling limits, the total metal concentrations in the effluent were found below the USEPA (below µg/L) guidelines. In general, the removal efficiencies for metals in LWWTP were ≥ 94%. The removal efficiencies of the anions were > 100% (Br-), 16.42% (Cl-), 78.89% (F-), 182.59% (NO3-), > 100% (NO2-), 51.81% (PO43-), and 67.01% (SO42-). In addition, Pierson correlation coefficients between the anions and cations, and implications for usage and suggested improvements of the treatment plants are proposed.


Assuntos
Chumbo , Metais Pesados , Texas , Chumbo/análise , Dióxido de Nitrogênio/análise , Monitoramento Ambiental , Ânions/análise , Metais Pesados/análise
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