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1.
Environ Sci Technol ; 58(15): 6595-6604, 2024 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-38573735

RESUMO

Meaningful interpretation of U isotope measurements relies on unraveling the impact of reduction mechanisms on the isotopic fractionation. Here, the isotope fractionation of hexavalent U [U(VI)] was investigated during its reductive mineralization by magnetite to intermediate pentavalent U [U(V)] and ultimately tetravalent U [U(IV)]. As the reaction proceeded, the remaining aqueous phase U [containing U(VI) and U(V)] systematically carried light isotopes, whereas in the bicarbonate-extracted solution [containing U(VI) and U(V)], the δ238U values varied, especially when C/C0 approached 0. This variation was interpreted as reflecting the variable relative contribution of unreduced U(VI) (δ238U < 0‰) and bicarbonate-extractable U(V) (δ238U > 0‰). The solid remaining after bicarbonate extraction included unextractable U(V) and U(IV), for which the δ238U values consistently followed the same trend that started at 0.3-0.5‰ and decreased to ∼0‰. The impact of PIPES buffer on isotopic fractionation was attributed to the variable abundance of U(V) in the aqueous phase. A few extremely heavy bicarbonate-extracted δ238U values were due to mass-dependent fractionation resulting from several hypothesized mechanisms. The results suggest the preferential accumulation of the heavy isotope in the reduced species and the significant influence of U(V) on the overall isotopic fractionation, providing insight into the U isotope fractionation behavior during its abiotic reduction process.


Assuntos
Óxido Ferroso-Férrico , Urânio , Bicarbonatos , Isótopos , Fracionamento Químico
2.
Methods Mol Biol ; 2794: 105-120, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38630224

RESUMO

Proteomics is a scientific field that aims to identify and characterize all proteins within a biological system, including their posttranslational modifications (PTMs), quantitative changes, and protein-protein interactions. Over the last two decades, proteomic approaches have been widely used in neuroscience research, providing multidimensional insights into the biology and pathology of the brain.Here, we present a basic protocol for profiling protein expression in the mouse brain, which involves total protein extraction, fractionation, digestion, and identification through liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). This method is compatible with many prevalent techniques used for protein quantitation, PTM analysis, and protein-protein interaction mapping.


Assuntos
Proteômica , Espectrometria de Massas em Tandem , Animais , Camundongos , Cromatografia Líquida , Encéfalo , Fracionamento Químico
3.
Sci Rep ; 14(1): 9182, 2024 Apr 22.
Artigo em Inglês | MEDLINE | ID: mdl-38649422

RESUMO

In order to obtain high yield pomelo peel pectin with better physicochemical properties, four pectin extraction methods, including hot acid extraction (HAE), microwave-assisted extraction (MAE), ultrasound-assisted extraction, and enzymatic assisted extraction (EAE) were compared. MAE led to the highest pectin yield (20.43%), and the lowest pectin recovery was found for EAE (11.94%). The physicochemical properties of pomelo peel pectin obtained by different methods were also significantly different. Pectin samples obtained by MAE had the highest methoxyl content (8.35%), galacturonic acid content (71.36%), and showed a higher apparent viscosity, thermal and emulsion stability. The pectin extracted by EAE showed the highest total phenolic content (12.86%) and lowest particle size (843.69 nm), showing higher DPPH and ABTS scavenging activities than other extract methods. The pectin extracted by HAE had the highest particle size (966.12 nm) and degree of esterification (55.67%). However, Fourier-transform infrared spectroscopy showed that no significant difference occurred among the different methods in the chemical structure of the extracted pectin. This study provides a theoretical basis for the industrial production of pomelo peel pectin.


Assuntos
Citrus , Ácidos Hexurônicos , Pectinas , Pectinas/química , Pectinas/isolamento & purificação , Citrus/química , Viscosidade , Tamanho da Partícula , Micro-Ondas , Espectroscopia de Infravermelho com Transformada de Fourier , Extratos Vegetais/química , Extratos Vegetais/isolamento & purificação , Fracionamento Químico/métodos , Fenômenos Químicos , Frutas/química , Antioxidantes/química , Antioxidantes/isolamento & purificação , Antioxidantes/farmacologia , Fenóis/análise , Fenóis/química , Fenóis/isolamento & purificação , Esterificação
4.
Environ Sci Technol ; 58(12): 5336-5346, 2024 Mar 26.
Artigo em Inglês | MEDLINE | ID: mdl-38472090

RESUMO

The re-emission and subsurface migration of legacy mercury (Hg) are not well understood due to limited knowledge of the driving processes. To investigate these processes at a decommissioned chlor-alkali plant, we used mercury stable isotopes and chemical speciation analysis. The isotopic composition of volatilized Hg(0) was lighter compared to the bulk total Hg (THg) pool in salt-sludge and adjacent surface soil with mean ε202HgHg(0)-THg values of -3.29 and -2.35‰, respectively. Hg(0) exhibited dichotomous directions (E199HgHg(0)-THg = 0.17 and -0.16‰) of mass-independent fractionation (MIF) depending on the substrate from which it was emitted. We suggest that the positive MIF enrichment during Hg(0) re-emission from salt-sludge was overall controlled by the photoreduction of Hg(II) primarily ligated by Cl- and/or the evaporation of liquid Hg(0). In contrast, O-bonded Hg(II) species were more important in the adjacent surface soils. The migration of Hg from salt-sludge to subsurface soil associated with selective Hg(II) partitioning and speciation transformation resulted in deep soils depleted in heavy isotopes (δ202Hg = -2.5‰) and slightly enriched in odd isotopes (Δ199Hg = 0.1‰). When tracing sources using Hg isotopes, it is important to exercise caution, particularly when dealing with mobilized Hg, as this fraction represents only a small portion of the sources.


Assuntos
Mercúrio , Mercúrio/análise , Esgotos/análise , Isótopos de Mercúrio/análise , Isótopos/análise , Solo/química , Fracionamento Químico , Monitoramento Ambiental
5.
Environ Geochem Health ; 46(4): 113, 2024 Mar 13.
Artigo em Inglês | MEDLINE | ID: mdl-38478134

RESUMO

The closure or relocation of many industrial enterprises has resulted in a significant number of abandoned polluted sites enriched in heavy metals to various degrees, causing a slew of environmental problems. Therefore, it is essential to conduct research on heavy metal contamination in the soil of industrial abandoned sites. In this study, soils at different depths were collected in a smelting site located in Hunan Province, China, to understand the Cr distribution, speciation and possible risks. The results revealed that the high-content Cr and Cr(VI) contamination centers were mainly concentrated near S1 (Sample site 1) and S5. The longitudinal migration law of chromium was relatively complex, not showing a simply uniform trend of decreasing gradually with depth but presenting a certain volatility. The vertical distribution characteristics of chromium and Cr(VI) pollution suggest the need for attention to the pollution from chromium slag in groundwater and deep soil layers. The results of different speciation of Cr extracted by the modified European Community Bureau of Reference (BCR) method showed that Cr existed primarily in the residual state (F4), with a relatively low content in the weak acid extraction state (F1). The correlation analysis indicated that Cr was affected by total Cr, pH, organic matter and total carbon during the longitudinal migration process. The RSP results revealed that the smelting site as a whole had a moderate level of pollution. Soil at depths of 2-5 m was more polluted than other soil layers. Consequently, it is necessary to treat the site soil as a whole, especially the subsoil layer (2-5 m). Health risk assessment demonstrated that the soil chromium pollution was hazardous to both adults and children, and the probability of carcinogenic and non-carcinogenic risk was relatively high in the latter group. As a result, children should be a group of special concern regarding the assessment and remediation of soil contaminated with Cr. This study can provide some insight into the contamination characteristics, ecological and health risks of chromium in contaminated soils and offer a scientific basis for the prevention and control of chromium pollution at abandoned smelting sites.


Assuntos
Metais Pesados , Poluentes do Solo , Adulto , Criança , Humanos , Solo/química , Poluentes do Solo/análise , Cromo/toxicidade , Cromo/análise , Metais Pesados/toxicidade , Metais Pesados/análise , China , Medição de Risco , Fracionamento Químico , Monitoramento Ambiental
6.
Ultrason Sonochem ; 105: 106852, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38518410

RESUMO

The "ultrasonic-assisted extraction (UAE)" method was utilized in this work to assess how different process parameters affected the yield and recovery of phenolic compounds from the leaf of Commiphora gileadensis, which is one of the medicinal plants with a variety of biological functions. Its leaf is used for a various of therapeutic applications, such as the treatment of bacterial infections, inflammation, and wound healing. The "One-Factor-At-a-Time (OFAT)" approach was employed to examine the impacts of various UAE process parameters on the process of extraction, which include time of extraction, sample/solvent ratio, ultrasonic frequency, and solvent (ethanol) concentration. The extracts were then investigated for the presence of several phytochemicals using analytical techniques such as "Gas Chromatography-Mass Spectroscopy (GC-MS)" and "Fourier Transform Infrared Spectroscopy (FTIR)" studies. The findings showed that the maximum extraction yield, the total phenolic content (TPC), and the total flavonoids content (TFC) of the ethanolic extract of the leaves of C. gileadensis using the UAE method were at 31.80 ± 0.41 %, 96.55 ± 2.81 mg GAE/g d.w. and 31.66 ± 2.01 mg QE/g d.w. accordingly under a procedure duration of 15 min, ultrasonic frequency of 20 kHz, solvent/sample ratio of 1:20 g/mL, and solvent concentration of 40 % v/v. The leaves extract of C. gileadensis included 25 phenolic compounds that were previously unreported, and GC-MS analysis confirmed their presence. Hence, it follows that the UAE technique can successfully extract the phytochemicals from C. gileadensis for a variety of therapeutic uses.


Assuntos
Fracionamento Químico , Commiphora , Fenóis , Folhas de Planta , Ondas Ultrassônicas , Commiphora/química , Folhas de Planta/química , Fenóis/isolamento & purificação , Fracionamento Químico/métodos , Extratos Vegetais/química , Extratos Vegetais/isolamento & purificação , Solventes/química
7.
Food Chem ; 448: 139061, 2024 Aug 01.
Artigo em Inglês | MEDLINE | ID: mdl-38537550

RESUMO

Recently, deep eutectic solvents (DES) have been extensively researched as a more biocompatible and efficient alternative to conventional solvents for extracting pigments from natural resources. The efficiency of DES extraction for the anthocyanin and carotenoid can be enhanced by microwave-assisted extraction (MAE) and/or ultrasound-assisted extraction (UAE) techniques. Apart from the extraction efficiency, the toxicity and recovery of the pigments and their bioavailability are crucial for potential applications. A plethora of studies have explored the extraction efficiency, toxicity, and recovery of pigments from various natural plant-based matrices using DES. Nevertheless, a detailed review of the deep eutectic solvent extraction of natural pigments has not been reported to date. Additionally, the toxicity, safety, and bioavailability of the extracted pigments, and their potential applications are not thoroughly documented. Therefore, this review is designed to understand the aforementioned concepts in using DES for anthocyanin and carotenoid extraction.


Assuntos
Antocianinas , Carotenoides , Solventes Eutéticos Profundos , Química Verde , Extratos Vegetais , Antocianinas/química , Antocianinas/isolamento & purificação , Carotenoides/química , Carotenoides/isolamento & purificação , Extratos Vegetais/química , Extratos Vegetais/isolamento & purificação , Solventes Eutéticos Profundos/química , Fracionamento Químico/métodos , Micro-Ondas
8.
Food Chem ; 448: 139104, 2024 Aug 01.
Artigo em Inglês | MEDLINE | ID: mdl-38547711

RESUMO

Legume proteins can be induced to form amyloid-like fibrils upon heating at low pH, with the exact conditions greatly impacting the fibril characteristics. The protein extraction method may also impact the resulting fibrils, although this effect has not been carefully examined. Here, the fibrillization of lentil protein prepared using various extraction methods and the corresponding fibril morphology were characterized. It was found that an acidic, rather than alkaline, protein extraction method was better suited for producing homogeneous, long, and straight fibrils from lentil proteins. During alkaline extraction, co-extracted phenolic compounds bound proteins through covalent and non-covalent interactions, contributing to the formation of heterogeneous, curly, and tangled fibrils. Recombination of isolated phenolics and proteins (from acidic extracts) at alkaline pH resulted in a distinct morphology, implicating a role for polyphenol oxidase also in modifying proteins during alkaline extraction. These results help disentangle the complex factors affecting legume protein fibrillization.


Assuntos
Lens (Planta) , Fenóis , Proteínas de Plantas , Lens (Planta)/química , Fenóis/química , Fenóis/isolamento & purificação , Proteínas de Plantas/química , Proteínas de Plantas/isolamento & purificação , Concentração de Íons de Hidrogênio , Extratos Vegetais/química , Extratos Vegetais/isolamento & purificação , Amiloide/química , Fracionamento Químico/métodos
9.
Ultrason Sonochem ; 105: 106856, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38554530

RESUMO

The residue remaining after oil extraction from grape seed contain abundant procyanidins. An ultrasonic-assisted enzyme method was performed to achieve a high extraction efficiency of procyanidins when the optimal extraction conditions were 8 U/g of cellulase, ultrasound power of 200 W, ultrasonic temperature of 50 ℃, and ultrasonic reaction time of 40 min. The effects of free procyanidins on both radical scavenging activity and thermal stability at 40, 60, and 80 ℃ of the procyanidins-loaded liposomal systems prepared by the ultrasonic-assisted method were discussed. The presence of procyanidins at concentrations ranging from 0.02 to 0.10 mg/mL was observed to be effective at inhibiting lipid oxidation by 15.15 % to 69.70 % in a linoleic acid model system during reaction for 168 h, as measured using the ferric thiocyanate method. The procyanidins-loaded liposomal systems prepared by the ultrasonic-assisted method were characterized by measuring the mean particle size and encapsulation efficiency. Moreover, the holographic plots showed that the effect-response points of procyanidins combined with α-tocopherol in liposomes were lower than the addition line and 95 % confidence interval limits. At the same time, there were significant differences between the theoretical IC50add value and the experimental IC50mix value. The interaction index (γ) of all combinations was observed to be less than 1. These results indicated that there was a synergistic antioxidant effect between procyanidins combined with α-tocopherol, which will show promising prospects in practical applications. In addition, particle size differentiation and morphology agglomeration were observed at different time points of antioxidant activity determination (0, 48, 96 h).


Assuntos
Antioxidantes , Lipossomos , Proantocianidinas , Proantocianidinas/isolamento & purificação , Proantocianidinas/química , Lipossomos/química , Antioxidantes/química , Antioxidantes/isolamento & purificação , Antioxidantes/farmacologia , Ondas Ultrassônicas , Vitis/química , Extrato de Sementes de Uva/química , Fracionamento Químico/métodos , Tamanho da Partícula , Temperatura , Sementes/química
10.
J Proteome Res ; 23(3): 881-890, 2024 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-38327087

RESUMO

Clinical diagnostics and microbiology require high-throughput identification of microorganisms. Sample multiplexing prior to detection is an attractive means to reduce analysis costs and time-to-result. Recent studies have demonstrated the discriminative power of tandem mass spectrometry-based proteotyping. This technology can rapidly identify the most likely taxonomical position of any microorganism, even uncharacterized organisms. Here, we present a simplified label-free multiplexing method to proteotype isolates by tandem mass spectrometry that can identify six microorganisms in a single 20 min analytical run. The strategy involves the production of peptide fractions with distinct hydrophobicity profiles using spin column fractionation. Assemblages of different fractions can then be analyzed using mass spectrometry. Results are subsequently interpreted based on the hydrophobic characteristics of the peptides detected, which make it possible to link each taxon identified to the initial sample. The methodology was tested on 32 distinct sets of six organisms including several worst-scenario assemblages-with differences in sample quantities or the presence of the same organisms in multiple fractions-and proved to be robust. These results pave the way for the deployment of tandem mass spectrometry-based proteotyping in microbiology laboratories.


Assuntos
Fracionamento Químico , Espectrometria de Massas em Tandem , Cromatografia Líquida
11.
Chemosphere ; 352: 141488, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38368960

RESUMO

By assessing the changes in stable isotope compositions within individual pesticide molecules, Compound Specific Isotope Analysis (CSIA) holds the potential to identify and differentiate sources and quantify pesticide degradation in the environment. However, the environmental application of pesticide CSIA is limited by the general lack of knowledge regarding the initial isotopic composition of active substances in commercially available formulations used by farmers. To address this limitation, we established a database aimed at cataloguing and disseminating isotopic signatures in commercial formulations to expand the use of pesticide CSIA. Our study involved the collection of 25 analytical standards and 120 commercial pesticide formulations from 23 manufacturers. Subsequently, 59 commercial formulations and 25 standards were extracted, and each of their active substance was analyzed for both δ13C (n = 84) and δ15N CSIA (n = 43). The extraction of pesticides did not cause significant isotope fractionation (Δ13C and Δ15N < 1‰). Incorporating existing literature data, stable carbon and nitrogen isotope signatures varied in a relatively narrow range among pesticide formulations for different pesticides (Δ13C and Δ15N < 10‰) and within different formulations for a single substance (Δ13C and Δ15N < 2‰). Overall, this suggests that pesticide CSIA is more suited for identifying pesticide transformation processes rather than differentiating pesticide sources. Moreover, an inter-laboratory comparison showed similar δ13C (Δ13C ≤ 1.2 ‰) for the targeted substances albeit varying GC-IRMS instruments. Insignificant carbon isotopic fractionation (Δ13C < 0.5‰) was observed after 4 years of storing the same pesticide formulations, confirming their viability for long-term storage at 4 °C and future inter-laboratory comparison exercises. Altogether, the ISOTOPEST database, in open access for public use and additional contributions, marks a significant advancement in establishing an environmentally relevant pesticide CSIA approach.


Assuntos
Praguicidas , Praguicidas/análise , Isótopos de Carbono/análise , Isótopos de Nitrogênio/análise , Fracionamento Químico
12.
Bioresour Technol ; 395: 130400, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38286169

RESUMO

The rational use of bamboo to make dissolving pulp can offer up new opportunities for cellulose production, alleviating wood scarcity. Bamboo contains a high content of non-fiber cells, which presents technical challenges in dissolving pulp production by the conventional process. In this study, a process concept of separating hemicelluloses is presented by fiber fractionation and purification for cleaner production of bamboo dissolving pulp: bamboo kraft pulp was fractionated into long-fiber and short-fiber fractions. The cellulose-rich long-fiber fraction was converted to dissolving pulp by further purification treatment with acid hydrolysis and cold caustic extraction. The hemicellulose-rich short-fiber fraction was used for papermaking. The laboratory results were confirmed by those from mill trials. The combined pulp yield (dissolving pulp + paper-grade pulp) reached 49 %, which was significantly higher than that of the conventional pre-hydrolysis kraft pulping process. Furthermore, the quality of dissolving pulp was higher due to inherently higher cellulose content of long-fiber fraction.


Assuntos
Celulose , Fracionamento Químico , Madeira , Hidrólise
13.
Chemosphere ; 351: 141198, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38218244

RESUMO

Copper and zinc are essential micronutrients that are potentially toxic when present in excess in soils. Their bioavailability depends on their speciation in soil, but this may vary with environmental conditions. Aeration and hence redox conditions, and organic matter amendments are among the factors likely to cause variation on metal fractionation. We have monitored the chemical fractionation of both native and added copper and zinc in a clay loam top soil during a 5-month laboratory incubation. The effects of aeration (moist soil or flooded) and addition of two organic matter amendments, alfalfa straw or leaf compost, were studied. Metal spike was more labile than legacy metal, and was slowly redistributed over the incubation period. Organic matter caused short-lived flushes of metals, attributed to metal chelation with soluble organic matter. This effect was greater for straw than for more stable compost. There was no evidence that added organic matter increased the capacity of soil organic matter to immobilise metal. Flooding solubilized soil metal (hydr)oxides, releasing legacy Cu and Zn, but with less effect on the capacity to immobilise metal spike. Effects of flooding and organic matter addition were not additive. Both metals appear to be precipitated as sulphides under reducing conditions, and accounted for in the acid soluble phase. Monitoring the dynamics of metal distribution gives a more comprehensive understanding of underlying processes than would a single measurement, and is closer to in campo conditions than slurry microcosms.


Assuntos
Metais Pesados , Poluentes do Solo , Cobre/química , Zinco , Metais Pesados/análise , Solo/química , Compostos Orgânicos , Poluentes do Solo/análise , Fracionamento Químico
14.
Appl Microbiol Biotechnol ; 108(1): 140, 2024 Jan 17.
Artigo em Inglês | MEDLINE | ID: mdl-38231394

RESUMO

Enzymes have become important tools in many industries. However, the full exploitation of their potential is currently limited by a lack of efficient and cost-effective methods for enzyme purification from microbial production. One technology that could solve this problem is foam fractionation. In this study, we show that diverse natural foam-stabilizing proteins fused as F-Tags to ß-lactamase, penicillin G acylase, and formate dehydrogenase, respectively, are able to mediate foaming and recovery of the enzymes by foam fractionation. The catalytic activity of all three candidates is largely preserved. Under appropriate fractionation conditions, especially when a wash buffer is used, some F-Tags also allow nearly complete separation of the target enzyme from a contaminating protein. We found that a larger distance between the F-Tag and the target enzyme has a positive effect on the maintenance of catalytic activity. However, we did not identify any particular sequence motifs or physical parameters that influenced performance as an F-tag. The best results were obtained with a short helical F-Tag, which was originally intended to serve only as a linker sequence. The findings of the study suggest that the development of molecular tags that enable the establishment of surfactant-free foam fractionation for enzyme workup is a promising method. KEY POINTS: • Foam-stabilizing proteins mediate activity-preserving foam fractionation of enzymes • Performance as an F-Tag is not restricted to particular structural motifs • Separation from untagged protein benefits from low foam stability and foam washings.


Assuntos
Fracionamento Químico , Penicilina Amidase , Formiato Desidrogenases , Indústrias , Tensoativos
15.
Int J Biol Macromol ; 259(Pt 1): 129186, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-38184047

RESUMO

Lignocellulosic biomass has emerged as a promising alternative with sustainable advantages for the production of a wide range of renewable products and value-added chemicals. In this study, a pretreatment strategy that use a fully recyclable acid hydrotrope (p-TsOH aqueous solution) to extract lignin and employ glyoxylic acid (GA) to stabilize lignin was proposed for biomass valorization toward multipurpose fractionation. 83.0 % of lignin was dissolved out by p-TsOH hydrotrope (80 wt%) with GA addition to form GA-stabilized product at 80 o C for 15 min. The stabilized lignin was subsequently used as an additive in the preparation of lignin-based suncream. Notably, the incorporation of 4 wt% lignin nanospheres into an SPF15 sunscreen yielded a measured SPF of 59.94. Furthermore, the depolymerization of uncondensed lignin into aromatic monomers yielded a high lignin-oil yield of 84.2 %. Additionally, direct heating of the pretreatment liquor facilitated the conversion of monosaccharides into furfural, achieving a desired yield of 53.7 % without the addition of any acid catalyst. The pretreatment also enhanced the enzymatic hydrolysis of glucan, resulting in a saccharification yield of 98.4 %. Moreover, short-term ultrasonication of the pretreated substrate yielded pulp suitable for papermaking. Incorporating 15 wt% fibers into the produced paper sheets led to a 5.3 % increase in tear index and a 25.4 % increase in tensile index. This study presents a viable pretreatment strategy for the multipurpose fractionation of lignocellulosic biomass, offering potential avenues for biomass valorization.


Assuntos
Lignina , Monossacarídeos , Lignina/metabolismo , Biomassa , Hidrólise , Fracionamento Químico
16.
Anal Bioanal Chem ; 416(5): 1239-1248, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-38193932

RESUMO

Hg isotope analysis in samples from background regions is constrained by the presence of low Hg concentration and therefore requires a pre-concentration method. Existing Hg pre-concentration methods are constrained by long sample processing time and limited sample loading capacity. Using foliar samples as a test case, an optimized Hg pre-concentration method is presented that involves the microwave-assisted digestion of samples for Hg isotope analysis with the addition of a pre-digestion step. Microwave-digested foliar samples and CRMs were transferred to an impinger, reduced with SnCl2, and collected in a 2.25 mL concentrated inverse aqua regia (3:1 HNO3:HCl, v/v). This resulted in an optimal acid concentration in the solution ideal for analysis on MC-ICP-MS. The time for purging with Hg-free N2 was optimized to 30 min and the efficiency of the pre-concentration method was tested using a combination of approaches. Tests performed on pure reagents and matrix of foliar samples spiked with 197Hg radiotracer showed recoveries averaging 99 ± 1.7% and 100 ± 3.0%, respectively. Mercury at concentrations as low as 1.83 ng g-1 was pre-concentrated by digesting aliquots of foliage samples in individual digestion vessels. Recoveries following their pre-concentration averaged 99 ± 6.0%, whereas recoveries of 95 ± 4.7% and 95 ± 2.5% were achieved for NIST SRM 1575a (pine needle) and reagents spiked with NIST SRM 3133, respectively. Analysis using multicollector-ICP-MS showed low fractionation of δ202Hg during sample pre-concentration with no significant mass-independent fractionation. The proposed method is a relatively simple and robust way to prepare Hg samples for Hg isotopic analysis and is suitable even for complex biological matrices.


Assuntos
Mercúrio , Isótopos de Mercúrio/análise , Mercúrio/análise , Isótopos , Fracionamento Químico
17.
Methods Mol Biol ; 2771: 1-5, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38285383

RESUMO

This procedure provides a comprehensive method for isolating double-stranded RNA (dsRNA) that relies on the different solubility of various nucleic acids in lithium chloride (LiC1). The approach offers several notable advantages including simplicity, avoidance of enzymatic treatments, and the ability to obtain relatively high yields of undegraded dsRNA over other conventional techniques. Moreover, it allows for the separation of different groups of cellular and viral nucleic acids from a single tissue sample. This method was further improved to increase the purity of dsRNA using plant tissues infected by RNA viruses.


Assuntos
Cloreto de Lítio , Ácidos Nucleicos , RNA de Cadeia Dupla , Fracionamento Químico , Solubilidade
18.
Int J Biol Macromol ; 254(Pt 3): 127948, 2024 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-37951432

RESUMO

Colloidal lignin particles (CLPs) have sparked various intriguing insights toward bio-polymeric materials and triggered many lignin-featured innovative applications. Here, we report a multi-solvent sequential fractionation methodology integrating green solvents of acetone, 1-butanol, and ethanol to fractionate industrial lignin for CLPs fabrication. Through a rationally designed fractionation strategy, multigrade lignin fractions with variable hydroxyl group contents, molecular weights, and high purity were obtained without altering their original chemical structures. CLPs with well-defined morphology, narrow size distribution, excellent thermal stability, and long-term colloidal stability can be obtained by rational selection of lignin fractions. We further elucidated that trace elements (S, N) were reorganized onto the near-surface area of CLPs from lignin fractions during the formation process in the form of -SO42- and -NH2. This work provides a sustainable and efficient strategy for refining industrial lignin into high-quality fractions and an in-depth insight into the CLPs formation process, holding great promise for enriching the existing libraries of colloidal materials.


Assuntos
Etanol , Lignina , Solventes/química , Lignina/química , Acetona , Fracionamento Químico/métodos
19.
Int J Biol Macromol ; 256(Pt 2): 128506, 2024 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-38040143

RESUMO

Hansen solubility parameters (HSPs) play a critical role in the majority of processes involving lignin depolymerization, separation, fractionation, and polymer blending, which are directly related to dissolution properties. However, the calculation of lignin HSPs is highly complicated due to the diversity of sources and the complexity of lignin structures. Despite their important role, lignin HSPs have been undervalued, attracting insufficient attention. This review summarizes the calculation methods for lignin HSPs and proposes a straightforward method based on lignin subunits. Furthermore, it highlights the crucial applications of lignin HSPs, such as identifying ideal solvents for lignin dissolution, selecting suitable solvents for lignin depolymerization and extraction, designing green solvents for lignin fractionation, and guiding the preparation of lignin-based composites. For instance, leveraging HSPs to design a series of solvents could potentially achieve sequential controllable lignin fractionation, addressing issues of low value-added applications of lignin resulting from poor homogeneity. Notably, HSPs serve as valuable tools for understanding the dissolution behavior of lignin. Consequently, we expect this review to be of great interest to researchers specializing in lignin and other macromolecules.


Assuntos
Lignina , Polímeros , Lignina/química , Solubilidade , Solventes/química , Fracionamento Químico
20.
Anal Chem ; 95(49): 18099-18106, 2023 12 12.
Artigo em Inglês | MEDLINE | ID: mdl-38047372

RESUMO

DNA size fractionation is an essential tool in molecular biology and is used to isolate targets in a mixture characterized by a broad molecular-weight distribution. Microfluidics was thought to provide the opportunity to create devices capable of enhancing and speeding up the classical fractionation processes. However, this conjecture met limited success due to the low mass or volume throughput of these technologies. We describe the µLAF (µ-laboratory for DNA fractionation) technology for DNA size selection based on the stacking of molecules on films of ∼100 µm in thickness with 105 cm-2 pores ∼2 µm in diameter. Size selection is achieved by controlling the regime of electrohydrodynamic migration through the temporal modulation of an electric field. This technology allows the processing of milliliter-scale samples containing a DNA mass of several hundreds of ng within ∼10 min and the selection of DNA in virtually any size window spanning 200 to 1000 bp. We demonstrate that one operation suffices to fractionate sheared genomic DNA in up to six fractions with collection efficiencies of ∼20-40% and enrichment factors of ∼1.5-3-fold. These performances compare favorably in terms of speed and versatility to those of the current standards.


Assuntos
Fracionamento Químico , DNA , Biologia Molecular , Eletricidade
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