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1.
Anal Biochem ; 692: 115574, 2024 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-38782251

RESUMEN

Ascorbic acid (AA), a prominent antioxidant commonly found in human blood serum, serves as a biomarker for assessing oxidative stress levels. Therefore, precise detection of AA is crucial for swiftly diagnosing conditions arising from abnormal AA levels. Consequently, the primary aim of this research is to develop a sensitive and selective electrochemical sensor for accurate AA determination. To accomplish this aim, we used a novel nanocomposite comprised of CeO2-doped ZnO adorned on biomass-derived carbon (CeO2·ZnO@BC) as the active nanomaterial, effectively fabricating a glassy carbon electrode (GCE). Various analytical techniques were employed to scrutinize the structure and morphology features of the CeO2·ZnO@BC nanocomposite, ensuring its suitability as the sensing nanomaterial. This innovative sensor is capable of quantifying a wide range of AA concentrations, spanning from 0.5 to 1925 µM in a neutral phosphate buffer solution. It exhibits a remarkable sensitivity of 0.2267 µA µM-1cm-2 and a practical detection limit of 0.022 µM. Thanks to its exceptional sensitivity and selectivity, this sensor enables highly accurate determination of AA concentrations in real samples. Moreover, its superior reproducibility, repeatability, and stability underscore its reliability and robustness for AA quantification.


Asunto(s)
Ácido Ascórbico , Carbono , Cerio , Técnicas Electroquímicas , Nanocompuestos , Óxido de Zinc , Ácido Ascórbico/análisis , Ácido Ascórbico/química , Ácido Ascórbico/sangre , Nanocompuestos/química , Óxido de Zinc/química , Técnicas Electroquímicas/métodos , Cerio/química , Carbono/química , Humanos , Biomasa , Electrodos , Límite de Detección
2.
Bioelectrochemistry ; 159: 108733, 2024 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-38761493

RESUMEN

It was previously reported that stress induces a cellular production of abscisic acid in plants, but no direct method shows the evidence. Here, an electrochemical microsensor involving an abscisic acid receptor PYL2 modified carbon fiber microelectrode was fabricated by self-assembly method, where the Cu2+ combined with the histidine tag of PYL2 on the surface of microelectrode was used as the detection probe, the mediated reaction between Cu+ and ferricyanide realized the amplification responses and provided the microsensor with a high sensitivity for detection of abscisic acid with a detection limit of 0.8 nM. With use of this microsensor, an increase of extracellular abscisic acid from single rice protoplast induced by sulfate, osmotic and salinity stress was real-time monitored. Direct measurement of free extracellular abscisic acid in single plant cells might offer important new insights into its role in plants challenged by abiotic stresses.


Asunto(s)
Ácido Abscísico , Microelectrodos , Oryza , Proteínas de Plantas , Protoplastos , Oryza/metabolismo , Oryza/química , Ácido Abscísico/metabolismo , Protoplastos/metabolismo , Proteínas de Plantas/metabolismo , Técnicas Biosensibles/métodos , Técnicas Biosensibles/instrumentación , Cobre/metabolismo , Técnicas Electroquímicas/métodos , Técnicas Electroquímicas/instrumentación , Ferricianuros/química , Ferricianuros/metabolismo
3.
J Hazard Mater ; 472: 134492, 2024 Jul 05.
Artículo en Inglés | MEDLINE | ID: mdl-38703687

RESUMEN

Nitrite plays a critical role in a variety of nitrification and denitrification processes in the nitrogen cycle. Due to the high surface energy, tendency to aggregate, and poor conductivity, current nitrite ZnS-based sensing platform could not meet the need of on-site nitrite detection in smart agriculture. In order to address these issues, the carboxylated carbon nanotube (CNT) was introduced to reduce the surface energy and prevented aggregation of ZnS, while ZnS-carboxylated CNT (ZnS-CNT) composite also provided excellent electrochemical conductivity. Furthermore, the introduction of phase transition BSA (PTB) created a three-dimensional porous conductive matrix without interfering with the mass transfer process of nitrite. The resulting sensing platform exhibited a linear detection range of 10 nM to 0.4 mM for nitrite, with a detection limit of 0.73 nM. And this sensing platform had the excellent antifouling ability to direct detection nitrite in real soil suspension. In addition, the sensing platform demonstrated remarkable resistance to interferences from pH variations, microbial presence, and organic pollutants that usually present in soil environment. Therefore, on-site detection of nitrite ions in soil environment was realized no needing complex pretreatments.

4.
Molecules ; 29(7)2024 Apr 05.
Artículo en Inglés | MEDLINE | ID: mdl-38611911

RESUMEN

An environmentally friendly and sustainable approach was adopted to produce a molecularly imprinted polymer (MIP) via electropolymerization, with remarkable electrochemical sensing properties, tested in tyrosine (tyr) detection. The 2,2'-bis(2,2'-bithiophene-5-yl)-3,3'-bithianaphtene (BT2-T4) was chosen as functional monomer and MIP electrosynthesis was carried out via cyclic voltammetry on low-volume (20 µL) screen-printed carbon electrodes (C-SPE) in ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ((BMIM) TFSI). An easy and rapid washing treatment allowed us to obtain the resulting MIP film, directly used for tyr electrochemical detection, carried out amperometrically. The sensor showed a linear response in the concentration range of 15-200 µM, with LOD of 1.04 µM, LOQ of 3.17 µM and good performance in selectivity, stability, and reproducibility. Tyrosine amperometric detection was also carried out in human plasma, resulting in a satisfactory recovery estimation. The work represents the first use of BT2-T4 as a functional monomer for the production of a molecularly imprinted polymer, with a green approach afforded by using a few microliters of a room temperature ionic liquid as an alternative to common organic solvents on screen-printed carbon electrodes, resulting in a valuable system that meets the green chemistry guidelines, which is today an essential criterion in both research and application field.

5.
Small Methods ; 8(7): e2301215, 2024 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-38678536

RESUMEN

Tailoring a material's surface with hierarchical structures from the micro- to the nanoscale is key for fabricating highly sensitive detection platforms. To achieve this, the fabrication method should be simple, inexpensive, and yield materials with a high density of surface features. Here, using benchtop fabrication techniques, gold surfaces with hierarchically structured roughness are generated for sensing applications. Hierarchical gold electrodes are prepared on pre-stressed polystyrene substrates via electroless deposition and amperometric pulsing. Electrodes fabricated using 1 mm H[AuCl4] and roughened with 80 pulses revealed the highest electroactive surface area. These electrodes are used for enzyme-free detection of glucose in the presence of bovine serum albumin and achieved a limit of detection of 0.36 mm, below glucose concentrations in human blood. The surfaces nanoroughened with 100 pulses also showed excellent surface-enhanced Raman scattering (SERS) response for the detection of rhodamine 6G, with an enhancement factor of ≈2 × 106 compared to detection in solution, and for the detection of a self-assembled monolayer of thiophenol, with an enhancement factor of ≈30 compared to the response from microstructured gold surfaces. It is envisioned that the simplicity and low fabrication cost of these gold-roughened structures will expedite the development of electrochemical and SERS sensing devices.

6.
Chemosphere ; 352: 141340, 2024 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-38301836

RESUMEN

Nanoarchitectured design of the metal sulfides with highly available surface and abundant electroactive centers and using them as electrocatalyst for fabricate the electrochemical sensors for the detection of hydrazine (N2H4) and hydrogen peroxide (H2O2) is challenging and desirable. Herein, Cu2O nanospheres powder is firstly prepared using chemical reduction of copper chloride and then drop-casted on the glassy carbon electrode (GCE) surface. In the next step, CoFeS nanoflakes are electrodeposited on Cu2O nanospheres by cyclic voltammetry method to form CoFeS/Cu2O nanocomposite as a detection platform for measuring N2H4 and H2O2. Accordingly, Cu2O nanospheres are not only used as substrate, but also guided the CoFeS nanoflakes to adhere to the electrode surface without need to any binder or conductive additive, which enhances the electrical conductivity of the sensing active materials. As the hydrazine sensor, the CoFeS/Cu2O/GCE displayed wide linear ranges (0.0001-0.021 mM and 0.021-1.771 mM), low detection limit (0.12 µM), very high sensitivities (103.33 and 21.23 mA mM-1 cm-2), and excellent selectivity. The as-made nanocomposite also exhibited low detection limit of 1.26 µM for H2O2 sensing with very high sensitivities (12.31 and 3.96 mA mM-1 cm-2) for linear ranges of 0.001-0.03 mM and 0.03-2.03 mM, respectively, and negligible response against interfering substances. The superior analytical performance of the CoFeS/Cu2O for N2H4 electro-oxidation and H2O2 electro-reduction can be attributed to structure stability, high electroactive surface area, and good availability to analyte species and electrolyte diffusion. Moreover, to examine the potency of the prepared nanocomposite in real applications, the seawater sample was analyzed and results display that the CoFeS/Cu2O/GCE can be utilized as a reliable and applicable platform for measuring N2H4 and H2O2.


Asunto(s)
Peróxido de Hidrógeno , Nanosferas , Peróxido de Hidrógeno/química , Cobre/química , Galvanoplastia , Carbono/química , Electrodos , Técnicas Electroquímicas/métodos
7.
Biosens Bioelectron ; 251: 116043, 2024 May 01.
Artículo en Inglés | MEDLINE | ID: mdl-38368643

RESUMEN

This article aims to present a comparative study of three polypyrrole-based molecularly imprinted polymer (MIP) systems for the detection of the recombinant severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) nucleocapsid protein (rN). The rN is known for its relatively low propensity to mutate compared to other SARS-CoV-2 antigens. The aforementioned systems include screen-printed carbon electrodes (SPCE) modified with gold nanostructures (MIP1), platinum nanostructures (MIP2), and the unmodified SPCE (MIP3), which was used for control. Pulsed amperometric detection (PAD) was employed as the detection technique, offering the advantage of label-free detection without the need for an additional redox probe. Calibration curves were constructed using the obtained data to evaluate the response of each system. Non-imprinted systems were also tested in parallel to evaluate the contribution of non-specific binding and assess the affinity sensor's efficiency. The analysis of calibration curves revealed that the AuNS-based MIP1 system exhibited the lowest contribution of non-specific binding and displayed a better fit with the chosen fitting model compared to the other systems. Further analysis of this system included determining the limit of detection (LOD) (51.2 ± 2.8 pg/mL), the limit of quantification (LOQ) (153.9 ± 8.3 pg/mL), and a specificity test using a recombinant receptor-binding domain of SARS-CoV-2 spike protein as a control. Based on the results, the AuNS-based MIP1 system demonstrated high specificity and sensitivity for the label-free detection of SARS-CoV-2 nucleocapsid protein. The utilization of PAD without the need for additional redox probes makes this sensing system convenient and valuable for rapid and accurate virus detection.


Asunto(s)
Técnicas Biosensibles , COVID-19 , Glicoproteína de la Espiga del Coronavirus , Humanos , SARS-CoV-2 , COVID-19/diagnóstico , Polímeros/química , Pirroles , Proteínas de la Nucleocápside/análisis
8.
Anal Chim Acta ; 1292: 342242, 2024 Mar 01.
Artículo en Inglés | MEDLINE | ID: mdl-38309852

RESUMEN

BACKGROUND: With the rapid growth of the demand for optically pure compounds in the fields of biology, medicine and stereospecific synthesis, it is of great importance to develop efficient, economical, simple enantioseparation and analysis methods. Open tubular capillary electrochromatography (OT-CEC) has attracted much attention in the field of chiral separation, but its column capacity and the sensitivity of common-used optical detection are relatively low. Zeolite beta nanomaterial is both enantioselective and size-selective, providing suitable chiral microenvironment for chiral recognition, and amperometric detection (AD) avoids the low sensitivity caused by the short optical path in optical detection to some extent. RESULTS: Zeolite beta nanomaterials with different particle sizes (25, 50 and 200 nm) were synthesized, and the morphology and structure were characterized by scanning electron microscopy and X-ray diffraction. Then, a novel chiral OT column was prepared by one-step method using zeolite beta nanomaterial as chiral stationary phase, and its separation performance was characterized by miniaturized CEC with AD (mini-CEC-AD) device. Under the optimum conditions, six groups of chiral drugs achieved baseline separation. Norepinephrine enantiomers were used for evaluating the inter-day, intra-day and inter-column reproducibility of the prepared open-tubular column. The relative standard deviations of migration time, peak area, resolution and selectivity factor were within 8.7 %. The limits of detection for norepinephrine enantiomers were 0.18 µg mL-1 (S/N = 3), and the average recoveries were in range of 96.7-105.0 %. This developed method has been successfully applied to the analysis of impurity enantiomer in potassium dichromate (+)-norepinephrine injection sample. SIGNIFICANCE: Zeolite beta nanomaterial was used as the stationary phase to prepare chiral OT columns for the first time, and this one-step preparation method is simple and easy. The introduction of zeolite beta enriches the types of chiral stationary phase materials in electrochromatographic columns, and mini-OT-CEC-AD system provides an alternative for fast enantioseparation of chiral compounds.

9.
Anal Biochem ; 688: 115464, 2024 May.
Artículo en Inglés | MEDLINE | ID: mdl-38244752

RESUMEN

This study describes the development of a highly sensitive amperometric biosensor for the analysis of phenolic compounds such as catechol. The biosensor architecture is based on the immobilization of tyrosinase (Tyr) on a screen-printed carbon electrode (SPE) modified with nanodiamond particles (ND), 1-butyl-3-methylimidazolium hexafluorophosphate (IL) and poly-l-lysine (PLL). Surface morphologies of the electrodes during the modification process were evaluated by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were used to investigate the electrochemical characteristics of the modified electrodes. Owing to the synergistic effect of the modification materials, the Tyr/PLL/ND-IL/SPE exhibited high sensitivity (328.2 µA mM-1) towards catechol with a wide linear range (5.0 × 10-8 - 1.2 × 10-5 M) and low detection limit (1.1 × 10-8 M). Furthermore, the method demonstrated good reproducibility and stability. The amperometric response of the biosensor towards other phenolic compounds such as bisphenol A, phenol, p-nitrophenol, m-cresol, p-cresol and o-cresol was also investigated. The analytical applicability of the biosensor was tested by the analysis of catechol in tap water. The results of the tap water analysis showed that the Tyr/PLL/ND-IL/SPE can be used as a practical and effective method for catechol determination.


Asunto(s)
Técnicas Biosensibles , Líquidos Iónicos , Nanodiamantes , Líquidos Iónicos/análisis , Polilisina , Reproducibilidad de los Resultados , Fenoles/análisis , Catecoles/análisis , Catecoles/química , Monofenol Monooxigenasa/química , Carbono/química , Agua , Técnicas Biosensibles/métodos , Electrodos , Técnicas Electroquímicas/métodos
10.
J Chromatogr A ; 1716: 464661, 2024 Feb 08.
Artículo en Inglés | MEDLINE | ID: mdl-38246068

RESUMEN

Lactose intolerance is a widespread condition, which prevents a large number of people from consuming dairy products as a part of their daily diet. It is estimated that an average of 65% of the global population is suffering from lactose intolerance. The global market for 'lactose-free' dairy products is rapidly growing and the criteria for 'lactose-free' labelled products are becoming stricter. To check the lactose contents in these products there is a need for fast, sensitive, and selective analytical method. A method is presented for fast and sensitive determination of lactose and its isomers using High-Performance Anion Exchange Chromatography in combination with Pulsed Amperometric Detection (HPAEC-PAD). The use of a new anion-exchange column, SweetSep™ AEX200, which is a strong anion-exchange column with highly monodisperse 5 µm particles, allowed the separation of all compounds of interest in less than 8 min with high resolution. A variety of dairy products were analyzed to demonstrate the versatility of the method.


Asunto(s)
Intolerancia a la Lactosa , Lactosa , Humanos , Lactosa/análisis , Cromatografía por Intercambio Iónico/métodos , Productos Lácteos/análisis , Aniones , Cromatografía Líquida de Alta Presión/métodos
11.
Int J Biol Macromol ; 254(Pt 2): 127903, 2024 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-37939751

RESUMEN

Glutamate (GLU) is a primary excitatory neurotransmitter, and its dysregulation is associated with several neurodegenerative disorders. A major challenge in GLU estimation is the existence of other biomolecules in the brain that could directly get oxidized at the electrode. Hence, highly selective electroenzymatic biosensors that enable rapid estimation of GLU are needed. Initially, a copolymer, poly(2-dimethylaminoethyl methacrylate- styrene) was synthesized through reversible addition-fragmentation chain transfer polymerization to noncovalently functionalize reduced graphene oxide (rGO), named DS-rGO. Glutamate oxidase macromolecule immobilized DS-rGO formed enzyme nanosheets, which was drop-coated over Prussian blue electrodeposited disposable electrodes to fabricate the GLU biosensor. The interconnectivity between the enzyme nanosheets and the Prussian blue endows the biosensor with enhanced conductivity and electrochemical activity. The biosensor exhibited a linearity: 3.25-250 µM; sensitivity: 3.96 µA mM-1 cm-2, and a limit of detection: 0.96 µM for GLU in the Neurobasal Medium. The biosensor was applied to an in vitro primary rat cortical model to discriminate GLU levels in Neurobasal Medium, before and after KCl mediated depolarization, which provides new insights for elucidating neuronal functioning in the brain.


Asunto(s)
Técnicas Biosensibles , Ácido Glutámico , Animales , Ratas , Ácido Glutámico/química , Ferrocianuros/química , Enzimas Inmovilizadas/química , Electrodos , Neuronas
12.
Mikrochim Acta ; 191(1): 47, 2023 12 22.
Artículo en Inglés | MEDLINE | ID: mdl-38133683

RESUMEN

Amino acid L-arginine (Arg), usually presented in food products and biological liquids, can serve both as a useful indicator of food quality and an important biomarker in medicine. The biosensors based on Arg-selective enzymes are the most promising devices for Arg assay. In this research, three types of amperometric biosensors have been fabricated. They exploit arginine oxidase (ArgO), recombinant arginase I (ARG)/urease, and arginine deiminase (ADI) coupled with the ammonium-chelating redox-active nanoparticles. Cadmium-copper nanoparticles (nCdCu) as the most effective nanochelators were used for the development of ammonium chemosensors and enzyme-coupled Arg biosensors. The fabricated enzyme/nCdCu-containing bioelectrodes show wide linear ranges (up to 200 µM), satisfactory storage stabilities (14 days), and high sensitivities (A⋅M-1⋅m-2) to Arg: 1650, 1700, and 4500 for ADI-, ArgO- and ARG/urease-based sensors, respectively. All biosensors have been exploited to estimate Arg content in commercial juices. The obtained data correlate well with the values obtained by the reference method. A hypothetic scheme for mechanism of action of ammonium nanochelators in electron transfer reaction on the arginine-sensing electrodes has been proposed.


Asunto(s)
Compuestos de Amonio , Técnicas Biosensibles , Ureasa/química , Arginina , Arginasa/metabolismo
13.
ACS Appl Mater Interfaces ; 15(47): 55183-55192, 2023 Nov 29.
Artículo en Inglés | MEDLINE | ID: mdl-37972391

RESUMEN

Paper has emerged as an excellent alternative to create environmentally benign disposable electrochemical sensing devices. The critical step to fabricating electrochemical sensors is making paper conductive. In this work, paper-based electrodes with a high electroactive surface area (ESA) were fabricated using a simple electroless deposition technique. The polymerization time of a polydopamine adhesion layer and the gold salt concentration during the electroless deposition step were optimized to obtain uniformly conductive paper-based electrodes. The optimization of these fabrication parameters was key to obtaining the highest ESA possible. Roughening factors (Rf) of 7.2 and 2.3 were obtained when cyclic voltammetry was done in sulfuric acid and potassium ferricyanide, respectively, demonstrating a surface prone to fast electron transfer. As a proof of concept, mercury detection was done through anodic stripping, achieving a limit of quantification (LOQ) of 0.9 ppb. By changing the metal deposition conditions, the roughness of the metalized papers could also be tuned for their use as surface-enhanced Raman scattering (SERS) sensors. Metallized papers with the highest SERS signal for thiophenol detection yielded a LOQ of 10 ppb. We anticipate that this method of fabricating nanostructured paper-based electrodes can accelerate the development of simple, cost-effective, and highly sensitive electrochemical and SERS sensing platforms.

14.
Biosensors (Basel) ; 13(10)2023 Oct 18.
Artículo en Inglés | MEDLINE | ID: mdl-37887129

RESUMEN

Melatonin (MT), a pineal gland hormone, regulates the sleep/wake cycle and is a potential biomarker for neurodegenerative disorders, depression, hypertension, and several cancers, including prostate cancer and hepatocarcinoma. The amperometric detection of MT was achieved using a sensor customized with ruthenium-incorporated carbon spheres (Ru-CS), possessing C- and O-rich catalytically active Ru surfaces. The non-covalent interactions and ion-molecule adducts between Ru and CS favor the formation of heterojunctions at the sensor-analyte interface, thus accelerating the reactions towards MT. The Ru-CS/Screen-printed carbon electrode (SPCE) sensor demonstrated the outstanding electrocatalytic oxidation of MT owing to its high surface area and heterogeneous rate constants and afforded a lower detection limit (0.27 µM), high sensitivity (0.85 µA µM -1 cm-2), and excellent selectivity for MT with the co-existence of crucial neurotransmitters, including norepinephrine, epinephrine, dopamine, and serotonin. High concentrations of active biomolecules, such as ascorbic acid and tyrosine, did not interfere with MT detection. The practical feasibility of the sensor for MT detection in pharmaceutical samples was demonstrated, comparable to the data provided on the product labels. The developed amperometric sensor is highly suitable for the quality control of medicines because of its low cost, simplicity, small sample size, speed of analysis, and potential for automation.


Asunto(s)
Melatonina , Rutenio , Carbono , Oxidación-Reducción , Epinefrina , Electrodos , Técnicas Electroquímicas
15.
Small ; : e2305333, 2023 Oct 19.
Artículo en Inglés | MEDLINE | ID: mdl-37857587

RESUMEN

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.

16.
Anal Biochem ; 681: 115334, 2023 Nov 15.
Artículo en Inglés | MEDLINE | ID: mdl-37774996

RESUMEN

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.

17.
J Pharm Biomed Anal ; 236: 115748, 2023 Nov 30.
Artículo en Inglés | MEDLINE | ID: mdl-37757546

RESUMEN

Enantioseparation has always been one of the research hotspots and difficulties in the field of modern separation science. In this work, a binary chiral electrophoretic separation system was constructed using deep eutectic solvents (DESs) coupled with beta-cyclodextrin derivatives based on capillary electrophoresis with amperometric detection system, and five groups of typical adrenergic receptor agonists (adrenaline, salbutamol, isoproterenol, norepinephrine and terbutaline) were selected as the model enantiomers. The effects of additive types and contents of DESs and cyclodextrins, and the pH value and concentration of the running buffer on the resolution of the selected chiral compounds were investigated in detail. The mechanism of DESs improving separation was explored preliminarily by means of UV spectrophotometry, which was further verified based on the comparison of single and mixed components of choline chlorine-urea DES. Under the optimum conditions, the relative standard deviations for inter-day and intra-day repeatability of the migration time, peak area and resolution for adrenaline and salbutamol were within 8.7%, and the limits of detection reached 0.030 µg mL-1 (S/N = 3). The recovery data were in the range of 96.3-118.7%. The developed methods have been applied for the analyses of (+)-adrenaline hydrochloride injection and (±)-salbutamol aerosol. This binary chiral electrophoretic separation system by CE-AD has high detection sensitivity and low analytical cost, providing an alternative for the separation and analysis of chiral drugs.


Asunto(s)
Ciclodextrinas , Disolventes Eutécticos Profundos , Agonistas Adrenérgicos , Ciclodextrinas/química , Albuterol/análisis , Epinefrina , Electroforesis Capilar/métodos , Estereoisomerismo
18.
Bioresour Technol ; 389: 129806, 2023 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-37769978

RESUMEN

Cellobiohydrolases are crucial for cellulose breakdown, but their efficiency on crystalline cellulose is hampered by limited access to single chain ends to initiate hydrolysis. As a result, they depend on enzymes like lytic polysaccharide monooxygenases (LPMOs), which directly target the crystalline cellulose surface. This study investigated how LPMO pretreatment affected the productive binding capacity of a Trichoderma longibrachiatum cellobiohydrolase, TlCBHI, on crystalline cellulose by applying an amperometric cellobiose dehydrogenase biosensor. After the 24-hour of LPMO pretreatment, the productive binding capacity of TlCBHI significantly increased in all reactions. However, with a shorter 5-hour LPMO pretreatment, minimal to no effect on productive binding capacity was observed. Of note, all LPMO reactions were inactivated around this time point. This delayed LPMO effect suggests that the improved binding capacity for cellulases does not directly result from cellulose chain cleavage by LPMOs but rather from the cellulose decrystallization following the oxidative cleavage.

19.
J Pharm Biomed Anal ; 235: 115646, 2023 Oct 25.
Artículo en Inglés | MEDLINE | ID: mdl-37595357

RESUMEN

Elevated urinary cystine levels are closely associated with the development of cystine stone. Therefore, the ability to rapidly and efficiently determine urinary cystine levels is crucial for physicians to manage patients with cystinuria or those undergoing cystine medication. In this study, an amperometric method employing a commercial screen-printed silver electrode was successfully established. The resulting calibration curve indicated a detection limit of 0.65 mg/dL. Satisfactory recoveries ranging from 89% to 109% were obtained for urine samples. The method was also effective for the quality control analysis of cystine in pharmaceutical tablets. The recovery of cystine from pharmaceutical tablets ranged from 98% to 101% using the developed method. This method enables the rapid and accurate determination of cystine in both urine samples and pharmaceutical tablets and provides valuable information for clinical diagnosis and pharmaceutical quality control.


Asunto(s)
Cistina , Plata , Humanos , Orina , Electrodos , Comprimidos
20.
J Chromatogr A ; 1706: 464264, 2023 Sep 13.
Artículo en Inglés | MEDLINE | ID: mdl-37562106

RESUMEN

Hierarchical porous zeolitic imidazolate framework­8 (HpZIF-8) have not only good chemical and thermal stability, but also pore structures of different sizes. In this work, HpZIF-8 supported hollow-fiber liquid-phase microextraction (HpZIF-8@HF-LPME) co-modified with tributyl phosphate and 2-nitroethyl benzene was firstly developed for purification and enrichment of nine typical phenolic pollutants followed by electrophoretic separation and amperometric detection (CE-AD). The key enrichment parameters were optimized by full factorial experimental and central composite designs. Under the optimum conditions, the maximum enrichment factors for the nine analytes were 479 (phenol), 249 (2-chlorophenol), 821 (4-chlorophenol), 1253 (3-methylphenol), 1376 (2,4-dichlorophenol), 1078 (2,4,6-trichlorophenol), 200 (pentachlorophenol), 614 (4-nitrophenol) and1827 times (bisphenol A), respectively. The limits of detection were 0.060-1.5 µg L-1 (S/N = 3) in real sample matrixes. This proposed method has been successfully applied to water samples with high ionic strength, and the average recoveries were in the range of 80.2-118.0%. This developed method of HpZIF-8@HF-LPME/CE-AD needs no desorption and derivatization, providing an alternative for monitoring typical phenolic pollutants in water samples.


Asunto(s)
Contaminantes Ambientales , Microextracción en Fase Líquida , Contaminantes Químicos del Agua , Contaminantes Ambientales/análisis , Porosidad , Fenoles/análisis , Electroforesis Capilar/métodos , Agua/análisis , Microextracción en Fase Líquida/métodos , Contaminantes Químicos del Agua/análisis
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