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1.
Small ; : e2305333, 2023 Oct 19.
Artigo em Inglês | MEDLINE | ID: mdl-37857587

RESUMO

The fabrication of a highly selective and ultrasensitive sulfite nanobiosensor based on a layered architectural fabrication aided by the encapsulation of sulfite oxidase (SOx) in Nafion (Naf) matrix on a multiwalled carbon nanotubes-polypyrrole (MWCNTs-PPy) composite decorated with platinum nanoparticles (PtNPs) is described. The MWCNTs are deposited in the inner layer on a Pt electrode during electropolymerization of pyrrole (Py), followed by decoration with a PtNPs layer and subsequent encapsulation of SOx with Naf in the third layer capped with a fourth thin PtNPs layer. Images obtained by field emission scanning electron microscopy (FESEM) reveal that high-density PtNPs are deposited onto the 3D nanostructured inner MWCNTs-PPy layer and the electrochemical behavior is investigated. A large surface area provided by the incorporation of MWCNTs in the composite and decoration with PtNPs enables increased SOx loading, SOx retention, and substantial improvement in sensing performance. The resulting layered PtNPs/SOx-Naf/PtNPs/MWCNTs-PPy nanobiosensor exhibits a fast response time (within 3 s), a linear calibration range of 20 nmm - 6 m with an excellent sensitivity of 71 µA mm-1  cm-2 and a detection limit of 5.4 nm. The nanobiosensor  was effective in discriminating against common interferants and  was successfully applied to sulfite determination in real samples.

2.
Electrophoresis ; 44(5-6): 492-500, 2023 03.
Artigo em Inglês | MEDLINE | ID: mdl-36413610

RESUMO

Dual detection concepts (DDCs) are becoming more and more popular in analytical chemistry. In this work, we describe a novel DDC for capillary electrophoresis (CE) consisting of an amperometric detector (AD) and a mass spectrometer (MS). This detector combination has a good complementarity as the AD exhibits high sensitivity, whereas the MS provides excellent selectivity. Both detectors are based on a destructive detection principle, making a serial detector arrangement impossible. Thus, for the realization of the DDC, the CE flow was divided into two parts with a flow splitter. The DDC was characterized in a proof-of-concept study with ferrocene derivates and a nonaqueous background electrolyte. We could show that splitting the CE flow was a suitable method for the instrumental realization of the DDC consisting of two destructive detectors. By lowering the height of the AD compared to the MS, it was possible to synchronize the detector responses. Additionally, for the chosen model system, we confirmed that the AD was much more reproducible and had lower limits of detection (LODs) than the MS. The LODs were identical for the DDC and the single-detection arrangements, indicating no sensitivity decrease due to the CE flow splitting. The DDC was successfully applied to determine the drug and doping agent trimetazidine.


Assuntos
Eletroforese Capilar , Espectrometria de Massas/métodos , Limite de Detecção , Eletroforese Capilar/métodos
3.
Anal Biochem ; 681: 115334, 2023 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-37774996

RESUMO

This work reports the profit of using a MOF compound for developing a sensitive electrochemical sensor to free chlorine detection in an aqueous solution. Co-MOF and FGO composites were synthesized and combined with the carbon paste (CP) to prepare an efficient electrochemical sensor with high sensing ability. The fabricated Co-MOF and FGO composites were characterized by SEM, EDX, FT-IR, and XRD techniques. Meanwhile, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were utilized to assess the electrochemical performance of the Co-MOF-FGO/CP modified electrode. Under the optimized condition, the amperometric detection showed that the reduction current of free chlorine increased linearly with a coefficient determination of 0.995 during its wide concentration range of 0.1-700 ppm. Also the detection limit (LOD) (S/N = 3) was 0.01 ppm. The selectivity of the sensor was tested with possible interferences, and satisfactory results were obtained. The proposed sensor was successfully used to determine the free chlorine in tap water and swimming pool water real samples. The results suggested that this proposed sensor could pave the way for developing the electrochemical sensor of free chlorine in aqueous media with MOFs.

4.
Mikrochim Acta ; 190(5): 195, 2023 04 27.
Artigo em Inglês | MEDLINE | ID: mdl-37106244

RESUMO

The synthesis of ultrasmall Ta2O5 nanoparticle anchored Pt atom using aspartic acid-functionalized graphene quantum dot (Asp-GQD) is reported. The Asp-GQD was combined with tantalic acid and chloroplatinic acid to rapidly form water-soluble Ta-Asp-GQD and Pt-Asp-GQD complex. Followed by thermal annealing at 900 °C in N2 to obtain Ta2O5-Asp-GQD-Pt. The study shows that the introduction of Asp-GQD as a chelating agent and p-type semiconductor achieves to the formation of ultrasmall Ta2O5 nanoparticle, PN junction at the interface and Pt single atom anchored on the surface of Ta2O5 nanocrystals. The unique structure realizes ultrahigh uricase activity and catalase activities of Ta2O5-Asp-GQD-Pt. The Ta2O5-Asp-GQD-Pt was used as the bifunctional sensing material for the construction of an electrochemical uric acid sensor. The differential pulse voltammetric current at 0.45 V linearly increases with the increase of uric acid concentration in the range 0.001-5.00 mM with the detection limit of 0.41 µM (S/N = 3). The sensor exhibits a much better sensitivity compared with the reported methods for the detection of uric acid. The proposed analytical method has been applied to the electrochemical detection of uric acid in human serum with a spiked recovery of 95-105%. The study also offers one way to design and synthesize multifunctional sensing materials with high catalytic activity.


Assuntos
Nanopartículas , Pontos Quânticos , Humanos , Ácido Úrico , Urato Oxidase/química , Catalase , Pontos Quânticos/química
5.
Sensors (Basel) ; 23(7)2023 Apr 04.
Artigo em Inglês | MEDLINE | ID: mdl-37050783

RESUMO

The aim of this electrochemical study was to ascertain which type of electrochemically deposited carbonyl functionalized polymer represents the most suitable electrode substrate for direct covalent immobilization of biological catalysts (enzymes). For this purpose, a triad of amperometric biosensors differing in the type of conductive polymers (poly-vanillin, poly-trans-cinnamaldehyde, and poly-4-hydroxybenzaldehyde) and in the functioning of selected enzymes (tyrosinase and alkaline phosphatase) has been compared for the biosensing of neurotransmitters (dopamine, epinephrine, norepinephrine, and serotonin) and phenyl phosphates (p-aminophenyl phosphate and hydroquinone diphosphate). The individual layers of the polymers were electrochemically deposited onto commercially available screen-printed carbon electrodes (type C110) using repetitive potential cycling in the linear voltammetric mode. Their characterization was subsequently performed by SEM imaging and attenuated total reflectance FTIR spectroscopy. Molecules of enzymes were covalently bonded to the free carbonyl groups in polymers via the Schiff base formation, in some cases even with the use of special cross-linkers. The as-prepared biosensors have been examined using cyclic voltammetry and amperometric detection. In this way, the role of the carbonyl groups embedded in the polymeric structure was defined with respect to the efficiency of binding enzymes, and consequently, via the final (electro)analytical performance.


Assuntos
Técnicas Biossensoriais , Técnicas Eletroquímicas , Animais , Bovinos , Técnicas Eletroquímicas/métodos , Polímeros/química , Técnicas Biossensoriais/métodos , Eletrodos , Espectroscopia de Infravermelho com Transformada de Fourier , Reprodutibilidade dos Testes
6.
Sensors (Basel) ; 23(3)2023 Feb 03.
Artigo em Inglês | MEDLINE | ID: mdl-36772727

RESUMO

Food contamination by aflatoxins is an urgent global issue due to its high level of toxicity and the difficulties in limiting the diffusion. Unfortunately, current detection techniques, which mainly use biosensing, prevent the pervasive monitoring of aflatoxins throughout the agri-food chain. In this work, we investigate, through ab initio atomistic calculations, a pyrrole-based Molecular Field Effect Transistor (MolFET) as a single-molecule sensor for the amperometric detection of aflatoxins. In particular, we theoretically explain the gate-tuned current modulation from a chemical-physical perspective, and we support our insights through simulations. In addition, this work demonstrates that, for the case under consideration, the use of a suitable gate voltage permits a considerable enhancement in the sensor performance. The gating effect raises the current modulation due to aflatoxin from 100% to more than 103÷104%. In particular, the current is diminished by two orders of magnitude from the µA range to the nA range due to the presence of aflatoxin B1. Our work motivates future research efforts in miniaturized FET electrical detection for future pervasive electrical measurement of aflatoxins.


Assuntos
Aflatoxinas , Técnicas Biossensoriais , Aflatoxina B1/análise , Aflatoxinas/análise , Contaminação de Alimentos/análise
7.
Environ Monit Assess ; 195(6): 630, 2023 May 02.
Artigo em Inglês | MEDLINE | ID: mdl-37129679

RESUMO

The standard method to determine chemical oxygen demand (COD) with K2Cr2O6 uses harmful chemicals, has a long analysis time, and cannot be used for on-site online monitoring. It is therefore necessary to find a fast, cheap, and harmless alternative. The amperometric determination of COD on boron-doped diamond (BDD) electrodes is a promising approach. However, to be a suitable alternative, the electrochemical method must at least be able to determine the COD of water samples independently of the contained substances. Therefore, the current signal as a function of various organic materials was investigated for the first time. It was shown that the height of the signal current depended on the type of organic matter in single-substance solutions and that this substance dependency increases with the amount of COD. Those findings could be explained by the mechanism proposed for this reaction, showing that the selectivity of the reaction depends on the ratio of the concentration of hydroxyl radicals and organic species. We give an outlook on how to improve the method in order to increase the linear working range and avoid signal variance and how to further explain the signal variance.


Assuntos
Monitoramento Ambiental , Poluentes Químicos da Água , Análise da Demanda Biológica de Oxigênio , Oxirredução , Boro , Eletrodos , Poluentes Químicos da Água/química , Oxigênio
8.
Anal Biochem ; 653: 114790, 2022 09 15.
Artigo em Inglês | MEDLINE | ID: mdl-35724942

RESUMO

Molecular size distribution of Haemophilus influenzae type b (Hib) conjugate vaccine is an important indicator for its immunogenicity and stability. Molecular size distribution was evaluated by High-Performance Protein Chromatography on Sepharose CL-4B column, and fractions were pooled. The use of high flow rate, incorporation of a calibration standard with the injected buffer and pooling method yielded a superior assay compared to conventional pharmacopeial method. The pools were analyzed for determination of distribution coefficient (KD) of 0.2 and 0.5 using two validated techniques: High Performance Anion Exchange Chromatography with pulsed amperometric detection (HPAEC-PAD) for ribitol determination and an optimized colorimetric assay for phosphorus determination. Linearity was achieved over range of 0.10-10.0 µg/mL and 1.0-8.0 µg/mL with LOD of 0.03 and 0.28 µg/mL for HPAEC and colorimetric assays, respectively. The developed assays were successfully applied in quality control monitoring of Hib conjugate vaccine. The optimized colorimetric method had shortened the analysis time to 25 min compared to 3.5 h for the European pharmacopeial assay by modifying the burning process. HPAEC stability results revealed 40% decrease in MSD after stressed storage conditions. The proposed assays offer a reliable and economic platform for monitoring the quality attributes of Hib for biopharma industry.


Assuntos
Vacinas Anti-Haemophilus , Lactose , Colorimetria , Vacinas Anti-Haemophilus/análise , Vacinas Anti-Haemophilus/química , Haemophilus influenzae , Vacinas Conjugadas
9.
Mikrochim Acta ; 189(5): 200, 2022 04 26.
Artigo em Inglês | MEDLINE | ID: mdl-35474402

RESUMO

Three-dimensional (3D) cobalt molybdate (CoMoO4) hierarchical nanoflake arrays on pencil graphite electrode (PGE) (CoMoO4/PGE) are actualized via one-pot hydrothermal technique. The morphological features comprehend that the CoMoO4 nanoflake arrays expose the 3D, open, porous, and interconnected network architectures on PGE. The formation and growth mechanisms of CoMoO4 nanostructures on PGE are supported with different structural and morphological characterizations. The constructed CoMoO4/PGE is operated as an electrocatalytic probe in enzyme-less electrochemical glucose sensor (ELEGS), confronting the impairments of cost- and time-obsessed conventional electrode polishing and catalyst amendment progressions and obliged the employment of a non-conducting binder. The wide-opened interior and exterior architectures of CoMoO4 nanoflake arrays escalate the glucose utilization efficacy, whilst the intertwined nanoflakes and graphitic carbon layers, respectively, of CoMoO4 and PGE articulate the continual electron mobility and catalytically active channels of CoMoO4/PGE. It jointly escalates the ELEGS concerts of CoMoO4/PGE including high sensitivity (1613 µA mM-1 cm-2), wide linear glucose range (0.0003-10 mM), and low detection limit (0.12 µM) at a working potential of 0.65 V (vs. Ag/AgCl) together with the good recovery in human serum. Thus, the fabricated CoMoO4/PGE extends exclusive virtues of modest electrode production, virtuous affinity, swift response, and excellent sensitivity and selectivity, exposing innovative prospects to reconnoitring the economically viable ELEGSs with binder-free, affordable cost, and expansible 3D electrocatalytic probes.


Assuntos
Grafite , Humanos , Cobalto , Eletrodos , Glucose , Grafite/química
10.
Mikrochim Acta ; 189(5): 188, 2022 04 11.
Artigo em Inglês | MEDLINE | ID: mdl-35404013

RESUMO

A laser-induced graphene (LIG) surface modified with Prussian blue (iron hexacyanoferrate) is demonstrated as a novel electrochemical sensing platform for the sensitive and selective detection of hydrogen peroxide. Electrochemical Prussian blue (PB) modification on porous graphene films engraved by infrared laser over flexible polyimide was accomplished. Scanning electron microscopy images combined with Raman spectra confirm the formation of porous graphene and homogenous electrodeposition of PB over this porous surface. Electrochemical impedance spectroscopy reveals a substantial decrease in the resistance to charge transfer values (from 395 to 31.4 Ω) after the PB insertion, which confirms the formation of a highly conductive PB-graphene composite. The synergistic properties of PB and porous graphene were investigated for the constant monitoring of hydrogen peroxide at 0.0 V vs. Ag|AgCl|KCl(sat.), under high-flow injections (166 µL s-1) confirming the high stability of the modified surface and fast response within a wide linear range (from 1 to 200 µmol L-1). Satisfactory detection limit (0.26 µmol L-1) and selectivity verified by the analysis of complex samples confirmed the excellent sensing performance of this platform. We highlight that the outstanding sensing characteristics of the developed sensor were superior in comparison with other PB-based or LIG-based electrochemical sensors reported for hydrogen peroxide detection.


Assuntos
Grafite , Técnicas Eletroquímicas/métodos , Eletrodos , Ferrocianetos , Grafite/química , Peróxido de Hidrogênio/análise , Lasers
11.
Mikrochim Acta ; 189(10): 385, 2022 09 20.
Artigo em Inglês | MEDLINE | ID: mdl-36125554

RESUMO

Cobalt hydroxide nanoparticles (Co(OH)2 NPs) were uniformly deposited on flexible carbon cloth substrate (Co(OH)2@CC) rapidly by a facile one-step electrodeposition, which can act as an enzyme-free glucose and uric acid sensor in an alkaline electrolyte. Compositional and morphological characterization were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDS), which confirmed the deposited nanospheres were Co(OH)2 nanoparticles (NPs). The electrochemical oxidation of glucose and uric acid at Co(OH)2@CC electrode was investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), differential pulse voltammetry (DPV), and chronoamperometry methods. The results revealed a remarkable electrocatalytic activity toward the single and simultaneous determination of glucose and uric acid at about 0.6 V and 0.3 V (vs. Ag/AgCl), respectively, which is attributed to a noticeable synergy effect between Co(OH)2 NPs and CC with good repeatability, satisfactory reproducibility, considerable long-term stability, superior selectivity, outstanding sensitivity, and wide linear detection range from 1 uM to 2 mM and 25 nM to 1.5 uM for glucose and UA, respectively. The detection limits were 0.36 nM for UA and 0.24 µM for glucose (S/N = 3). Finally, the Co(OH)2@CC electrode was utilized for glucose and uric acid determination in human blood samples and satisfying results were obtained. The relative standard derivations (RSDs) for glucose and UA were in the range 6 to 14% and 0 to 3%, respectively. The recovery ranges for glucose an UA were 97 to 103% and 95 and 101%, respectively. These features make the novel Co(OH)2@CC sensor developed by a low-cost, efficient, and eco-friendly preparation method a potentially practical candidate for application to biosensors.


Assuntos
Carbono , Nanopartículas , Carbono/química , Técnicas Eletroquímicas/métodos , Glucose , Humanos , Nanopartículas/química , Reprodutibilidade dos Testes , Ácido Úrico
12.
Mikrochim Acta ; 189(1): 46, 2022 01 05.
Artigo em Inglês | MEDLINE | ID: mdl-34985727

RESUMO

Wearable film-based smart biosensors have been developed for real-time biomolecules detection. Particularly, interfacial co-assembly of reduced graphene oxide-prussian blue (PB-RGO) film through electrostatic interaction has been systematically studied by controllable pH values, achieving optimal PB-RGO nanofilms at oil/water (O/W) phase interface driven by minimization of interfacial free energy for wearable biosensors. As a result, as-prepared wearable biosensors of PB-RGO film could be easily woven into fabrics, exhibiting excellent glucose sensing performance in amperometric detection with a sensitivity of 27.78 µA mM-1 cm-2 and a detection limit of 7.94 µM, as well as impressive mechanical robustness of continuously undergoing thousands of bending or twist. Moreover, integrated wearable smartsensing system could realize remotely real-time detection of biomarkers in actual samples of beverages or human sweat via cellphones. Prospectively, interfacial co-assembly engineering driven by pH-induced electrostatic interaction would provide a simple and efficient approach for acquiring functional graphene composites films, and further fabricate wearable smartsensing devices in health monitoring fields.


Assuntos
Técnicas Biossensoriais , Técnicas Eletroquímicas , Ferrocianetos/química , Glucose/análise , Grafite/química , Dispositivos Eletrônicos Vestíveis , Atenção à Saúde , Humanos , Tamanho da Partícula , Propriedades de Superfície
13.
Sensors (Basel) ; 22(9)2022 May 02.
Artigo em Inglês | MEDLINE | ID: mdl-35591157

RESUMO

A porous layer of copper was formed on the surface of screen-printed carbon electrodes via the colloidal crystal templating technique. An aqueous suspension of monodisperse polystyrene spheres of 500 nm particle diameter was drop-casted on the carbon tracks printed on the substrate made of alumina ceramic. After evaporation, the electrode was carefully dipped in copper plating solution for a certain time to achieve a sufficient penetration of solution within the polystyrene spheres. The metal was then electrodeposited galvanostatically over the self-assembled colloidal crystal. Finally, the polystyrene template was dissolved in toluene to expose the porous structure of copper deposit. The morphology of porous structures was investigated using scanning electron microscopy. Electroanalytical properties of porous copper film electrodes were evaluated in amperometric detection of selected saccharides, namely glucose, fructose, sucrose, and galactose. Using hydrodynamic amperometry in stirred alkaline solution, a current response at +0.6 V vs. Ag/AgCl was recorded after addition of the selected saccharide. These saccharides could be quantified in two linear ranges (0.2-1.0 µmol L-1 and 4.0-100 µmol L-1) with detection limits of 0.1 µmol L-1 glucose, 0.03 µmol L-1 fructose, and 0.05 µmol L-1 sucrose or galactose. In addition, analytical performance of porous copper electrodes was ascertained and compared to that of copper film screen-printed carbon electrodes, prepared ex-situ by the galvanostatic deposition of metal in the plating solution. After calculating the current densities with respect to the geometric area of working electrodes, the porous electrodes exhibited much higher sensitivity to changes in concentration of analytes, presumably due to the larger surface of the porous copper deposit. In the future, they could be incorporated in detectors of flow injection systems due to their long-term mechanical stability.


Assuntos
Carbono , Cobre , Carbono/química , Cobre/química , Eletrodos , Frutose , Galactose , Glucose , Poliestirenos , Sacarose
14.
Anal Bioanal Chem ; 413(11): 3017-3026, 2021 May.
Artigo em Inglês | MEDLINE | ID: mdl-33635387

RESUMO

The long-term consumption of food with pesticide residues has harmful effects on human health and the demand for pesticide detection technology tends to be miniaturized and instant. To this end, we demonstrated the first application of indirectly detecting two carbamate pesticides, metolcarb and carbaryl, by gold nanoparticle-modified indium tin oxide electrode in dual-channel microchip electrophoresis and amperometric detection (ME-AD) system. m-Cresol and α-naphthol were obtained after pesticide hydrolysis in alkaline solution, and then separated and detected by ME-AD. Parameters including the detection potential and running buffer concentration and pH were optimized to improve the detection sensitivity and separation efficiency. Under the optimal conditions, the two analytes were completely separated within 80 s. m-Cresol and α-naphthol presented a wide linear range from 1 to 100 µM, with limits of detection of 0.16 µM and 0.34 µM, respectively (S/N = 3). Moreover, the reliability of this system was demonstrated by analyzing metolcarb and carbaryl in spiked vegetable samples.


Assuntos
Carbamatos/análise , Técnicas Eletroquímicas/métodos , Eletroforese em Microchip/métodos , Resíduos de Praguicidas/análise , Limite de Detecção , Padrões de Referência , Reprodutibilidade dos Testes , Verduras/química
15.
Anal Bioanal Chem ; 413(3): 799-811, 2021 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-32474723

RESUMO

Early diagnosis in primary care settings can increase access to therapies and their efficiency as well as reduce health care costs. In this context, we report in this paper the development of a disposable immunoplatform for the rapid and simultaneous determination of two protein biomarkers recently reported to be involved in the pathological process of neurodegenerative disorders (NDD), tau protein (tau), and TAR DNA-binding protein 43 (TDP-43). The methodology involves implementation of a sandwich-type immunoassay on the surface of dual screen-printed carbon electrodes (dSPCEs) electrochemically grafted with p-aminobenzoic acid (p-ABA), which allows the covalent immobilization of a gold nanoparticle-poly(amidoamine) (PAMAM) dendrimer nanocomposite (3D-Au-PAMAM). This scaffold was employed for the immobilization of the capture antibodies (CAbs). Detector antibodies labeled with horseradish peroxidase (HRP) and amperometric detection at - 0.20 V (vs. Ag pseudo-reference electrode) using the H2O2/hydroquinone (HQ) system were used. The developed methodology exhibits high sensitivity and selectivity for determining the target proteins, with detection limits of 2.3 and 12.8 pg mL-1 for tau and TDP-43, respectively. The simultaneous determination of tau and TDP-43 was accomplished in raw plasma samples and brain tissue extracts from healthy individuals and NDD-diagnosed patients. The analysis can be performed in just 1 h using a simple one-step assay protocol and small sample amounts (5 µL plasma and 2.5 µg brain tissue extracts). Graphical abstract.


Assuntos
Proteínas de Ligação a DNA/metabolismo , Dendrímeros/química , Ouro/química , Imunoensaio/métodos , Nanopartículas Metálicas/química , Doenças Neurodegenerativas/diagnóstico , Poliaminas/química , Proteínas tau/metabolismo , Biomarcadores/sangue , Biomarcadores/metabolismo , Encéfalo/metabolismo , Estudos de Casos e Controles , Proteínas de Ligação a DNA/sangue , Eletrodos , Humanos , Doenças Neurodegenerativas/sangue , Doenças Neurodegenerativas/metabolismo , Proteínas tau/sangue
16.
Anal Bioanal Chem ; 413(21): 5517-5527, 2021 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-34286356

RESUMO

To achieve the measurement reliability of monosaccharides used as diagnostic markers in clinical fields, it is essential to establish certified reference materials (CRMs). The purpose of this study is to develop a serum CRM by adopting high-performance anion-exchange chromatography with pulsed amperometric detection (HPAEC-PAD) as a new candidate reference measurement procedure for the measurement of glucose and galactose, common diagnostic markers of diabetes and galactosemia, respectively. Using various monosaccharides as internal standards, the accuracy of the HPAEC-PAD method was tested by measuring glucose CRM following treatment with three different deproteinization methods: ultrafiltration, protein precipitation by trichloroacetic acid (TCA), and protein precipitation by acetonitrile. Results showed that ultrafiltration and 5% TCA provided good accuracy with every tested monosaccharide as the internal standard. Accordingly, serum samples in this study were treated by ultrafiltration after adding 2-deoxy-D-glucose and arabinose, which were selected as internal standards for galactose and glucose, respectively. Both intra- and inter-day recovery tests showed good precision and accuracy within 2%. From the serum CRM batches prepared at two levels, 11 units were analyzed by exact-matched calibration methods, and the mass fractions of galactose and glucose were determined via HPAEC-PAD. The between-unit relative standard deviations were not more than 1.5%, showing homogeneity. The expanded uncertainties (%) of galactose and glucose for both levels were less than 3.6% and 2.3% at 95% confidence. The HPAEC-PAD method presented in this study can significantly improve the accuracy and precision of simultaneous monosaccharide analysis, allowing for the development of further serum CRMs for monosaccharides. Graphical abstract.


Assuntos
Cromatografia por Troca Iônica/métodos , Monossacarídeos/sangue , Glicemia/análise , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida de Alta Pressão/normas , Cromatografia por Troca Iônica/normas , Galactose/sangue , Humanos , Limite de Detecção , Padrões de Referência , Reprodutibilidade dos Testes
17.
J Sep Sci ; 44(11): 2221-2233, 2021 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-33811795

RESUMO

The analysis of complex oligosaccharide mixtures remains a challenge in the field of analytical chemistry. In this work, two commercial galacto-oligosaccharides samples were characterized using high-performance anion exchange chromatography coupled to mass spectrometry. The isomeric oligosaccharides were resolved with high resolution. The structures of the individual isomers with a degree of polymerization up to 6 were analyzed using targeted selected ion monitoring with data-dependent tandem mass spectrometry, with additional in-source collision-induced dissociation.


Assuntos
Galactose/análise , Oligossacarídeos/análise , Cromatografia por Troca Iônica , Espectrometria de Massas em Tandem
18.
Mikrochim Acta ; 188(2): 48, 2021 01 23.
Artigo em Inglês | MEDLINE | ID: mdl-33486540

RESUMO

A dense  zeolitic imidazolate framework (ZIF) nanosheet is for the first time molded by reduced graphite oxide (RGO) and graphitic carbon nitride (g-C3N4) to fabricate an original 2D/2D/2D heterojunction (ZIF/g-C3N4/RGO nanohybrid), which is pipetted onto carbon cloth electrode (CCE) (ZIF/g-C3N4/RGO/CCE) as an electrochemical sensor. Profiting from the renowned synergistic and coupling effects, the resulting nanohybrid endows excellent electrocatalytic activity towards hydrazine. Amperometric detection reveals that the hybrid sensor possesses a low detection limit of 32 nM (S/N = 3) in a monitoring range of 0.0001 to 1.0386 mM, along with a high sensitivity 93.71 µA mM-1 cm-2. Importantly, the minimum detection concentration of hydrazine in the actual sample is lower than the maximum allowable limit of the World Health Organization (WHO) and has high reproducibility (RSD = 4.82%). As expected, the high sensing capability  of ZIF/g-C3N4/RGO combines the advantages of abundant surface-active sites and high conductivity along with 2D interfaces between ZIF, g-C3N4, and RGO nanosheets. This study provides a promising to expand 2D-based ternary nanojunction as a bridge for promoting sensing performance.Graphical abstract.


Assuntos
Hidrazinas/análise , Nanocompostos/química , Poluentes Químicos da Água/análise , Água Potável/análise , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/métodos , Eletrodos , Grafite/química , Água Subterrânea/análise , Hidrazinas/química , Limite de Detecção , Estruturas Metalorgânicas/química , Compostos de Nitrogênio/química , Oxirredução , Reprodutibilidade dos Testes , Esgotos/análise , Poluentes Químicos da Água/química
19.
Mikrochim Acta ; 188(11): 375, 2021 10 12.
Artigo em Inglês | MEDLINE | ID: mdl-34635945

RESUMO

A novel kind of chiral open-tubular (OT) column was established with homochiral zeolitic imidazolate framework-8 nanomaterials using L-histidine as the chiral carbon center (L-His-ZIF-8). The morphologies of L-His-ZIF-8 nanoparticles and chiral OT column were characterized by scanning electron microscopy. The effects of L-His-ZIF-8 concentrations, pH values, and concentrations of the running buffer on the resolution of the selected chiral compounds were investigated based on miniaturized capillary electrochromatography with amperometric detection system (mini-CEC-AD), respectively. The separation performances of the prepared L-His-ZIF-8@OT chiral columns were explored under the optimal conditions, and the RSDs of run-to-run, day-to-day, and column-to-column reproducibility were less than 6.7% using salbutamol raceme as the model enantiomers. The prepared chiral OT columns have been successfully applied to the enantioseparation of one pair of amino acid enantiomers, two pairs of racemic drugs, and three pairs of neurotransmitter enantiomers. Under the optimum conditions, the prepared OT columns were applied to real-world sample analysis of salbutamol aerosol. The limits of detection of salbutamol raceme were 0.90 µg·mL-1 (S/N = 3), and the recovery was 80.4-82.7%. The assay results indicated that this kind of chiral OT column modified with homochiral L-His-ZIF-8 possesses good reproducibility and stability. This developed mini-OT-CEC-AD system has some attractive characteristics of sensitivity and low cost, providing a potential way for the separation of chiral compounds.


Assuntos
Eletrocromatografia Capilar
20.
Int J Mol Sci ; 22(9)2021 May 10.
Artigo em Inglês | MEDLINE | ID: mdl-34068596

RESUMO

The review focuses on the overview of electrochemical sensors based on molecularly imprinted polymers (MIPs) for the determination of uric acid. The importance of robust and precise determination of uric acid is highlighted, a short description of the principles of molecular imprinting technology is presented, and advantages over the others affinity-based analytical methods are discussed. The review is mainly concerned with the electro-analytical methods like cyclic voltammetry, electrochemical impedance spectroscopy, amperometry, etc. Moreover, there are some scattered notes to the other electrochemistry-related analytical methods, which are capable of providing additional information and to solve some challenges that are not achievable using standard electrochemical methods. The significance of these overviewed methods is highlighted. The overview of the research that is employing MIPs imprinted with uric acid is mainly targeted to address these topics: (i) type of polymers, which are used to design uric acid imprint structures; (ii) types of working electrodes and/or other parts of signal transducing systems applied for the registration of analytical signal; (iii) the description of the uric acid extraction procedures applied for the design of final MIP-structure; (iv) advantages and disadvantages of electrochemical methods and other signal transducing methods used for the registration of the analytical signal; (vi) overview of types of interfering molecules, which were analyzed to evaluate the selectivity; (vi) comparison of analytical characteristics such as linear range, limits of detection and quantification, reusability, reproducibility, repeatability, and stability. Some insights in future development of uric acid sensors are discussed in this review.


Assuntos
Técnicas Biossensoriais , Eletroquímica , Polímeros Molecularmente Impressos/química , Ácido Úrico/isolamento & purificação , Humanos , Ácido Úrico/química
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