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1.
Analyst ; 148(11): 2544-2552, 2023 May 30.
Artigo em Inglês | MEDLINE | ID: mdl-37144556

RESUMO

Antibiotic residues pose a serious threat to ecosystems and food safety. Developing convenient, visual, and on-site detection methods is therefore in high demand and has a practical purpose. In this work, a near-infrared (NIR) fluorescent probe with an analysis platform based on a smartphone has been constructed for quantitative and on-site detection of metronidazole (MNZ). CdTe quantum dots with NIR emission at 710 nm (QD710) were prepared by using a simple hydrothermal method and showed good properties. A spectral overlap between absorption of MNZ and excitation of QD710 resulted in an effective inner filter effect (IFE) between QD710 and MNZ. Because of the IFE, the fluorescence of QD710 decreased gradually with increasing concentrations of MNZ. Based on the fluorescence response, quantitative detection and visualization of MNZ was achieved. NIR fluorescence analysis and the special IFE between probe and target can improve sensitivity and selectivity for MNZ. Additionally, these were also utilized for quantitative detection of MNZ in real food samples and the results were reliable and satisfactory. Meanwhile, a portable visual analysis platform in a smartphone was constructed for on-site analysis of MNZ, which can be used as an alternative method for detection of MNZ residues in situations with limited instrumental conditions. Therefore, this work provides a convenient, visual, and real-time analysis method for detection of MNZ and the analysis platform shows great potential for commercialization.


Assuntos
Compostos de Cádmio , Pontos Quânticos , Metronidazol/análise , Corantes Fluorescentes/química , Compostos de Cádmio/química , Ecossistema , Smartphone , Pontos Quânticos/química , Telúrio/química , Carbono/química , Limite de Detecção
2.
Environ Res ; 216(Pt 3): 114643, 2023 01 01.
Artigo em Inglês | MEDLINE | ID: mdl-36341789

RESUMO

The spread of antibiotic resistant genes has become a serious global concern. Thus, the development of efficient antibiotic monitoring systems to reduce their environmental risks is of great importance. Here, a potent electrochemical sensor was fabricated to detect metronidazole (MNZ) on the basis of green synthesis of Fe3O4 nanoparticles (NPs) using Sambucus ebulus L. leaves alcoholic plant extract as a safe and impressive reducing and stabilizing agent. Several analyses such as X-ray diffraction (XRD), Fourier transform infrared spectrophotometer (FTIR), thermogravimetric analysis (TGA), field emission scanning electron microscope (FESEM), energy dispersive X-ray spectroscopy (EDX), and dynamic light scattering (DLS) confirmed the production of homogeneous, monodisperse, regular, and stable magnetite NPs with a spherical morphology. The as-prepared Fe3O4NPs were afterwards applied to evaluate the electrochemical activity of MNZ by merging them with graphene nanosheets (GR NSs) on the glassy carbon electrode (GCE). The GR/Fe3O4NPs/GCE represented extraordinary catalytic activity toward MNZ with two dynamic ranges of 0.05-5 µM and 5-120 µM, limit of detection (LOD) of 0.23 nM, limit of quantification (LOQ) of 0.76 nM, and sensitivity of 7.34 µA µM-1 cm-2. The fabricated sensor was further employed as a practical tool for electrochemical detection of MNZ in real aqueous samples.


Assuntos
Nanopartículas de Magnetita , Metronidazol , Metronidazol/análise , Técnicas Eletroquímicas/métodos , Antibacterianos , Nanopartículas de Magnetita/química , Carbono/química , Fenômenos Magnéticos
3.
J Environ Manage ; 347: 119104, 2023 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-37793292

RESUMO

Current study covers the preparation and application of a commercial modified lead oxide battery electrode (LBE) in electrochemical oxidation (ECO) of metronidazole (MNZ) in an aqueous phase. Modified electrode is prepared by doping of bimetal-oxide (Fe and Zn) nanoparticles (NPs) & single metal-oxide (Fe/Zn) on bagasse-waste carbon (bwc) which is further coated on LBE. The modified LBE electrode surface was examined for metal-oxide NPs through X-ray diffraction analysis (XRD). Different electrodes are prepared by varying combinations of two metal-oxide based on molar ratio and tested for electrochemical characterization and MNZ removal test. Based on large oxygen evolution potential in a linear sweep volumetry (LSV) analysis and high MNZ removal rate, the best electrode has been represented as Fe1:Co2-bwc/LBE which contains Fe & Co molar ratio of 1:2. Moreover, equilibrium attained at faster rate in degradation process of MNZ, where pseudo first order kinetics of 2.29 × 10-2 min-1 was obtained under optimized condition of (MNZ:100 mg/L, pH:7, CD: 30 mA/cm2 and electrolyte: 0.05 M Na2SO4). Maximum MNZ removal, total organic carbon removal (TOC), mineralization current efficiency (MCE) & energy consumption (EC) of 98.7%, 85.3%, 62.2% & 96.143 kW h/kg-TOC removed are found in 180 min of treatment time for Fe1:Co2-bwc/LBE electrode. Accelerated service life test confirms that the stability of modified electrode is enhanced by 1.5 times compared to pristine LBE. Repeatability test confirms that modified LBE (Fe1:Co2-bwc/LBE) can be utilized up to 3 times.


Assuntos
Metronidazol , Poluentes Químicos da Água , Metronidazol/análise , Metronidazol/química , Carbono , Dióxido de Carbono/análise , Chumbo , Óxidos , Oxirredução , Eletrodos , Poluentes Químicos da Água/química
4.
J Environ Manage ; 342: 118161, 2023 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-37210822

RESUMO

There are growing concerns about the toxicity of metronidazole (MNZ) antibiotics in wastewater, which must be removed. This study used AgN/MOF-5 (1:3) to investigate the adsorptive removal of MNZ antibiotics from wastewater. Green synthesis of Ag-nanoparticles was from Argemone mexicana leaf aqueous extract blended with the synthesized MOF-5 in 1:3 by proportion. The adsorption materials were characterized by scanning electron microscope (SEM), N2 adsorption-desorption analysis, X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The surface area increased due to the appearance of micropores. Besides, the efficiency of AgN/MOF-5 (1:3) for MNZ removal was evaluated by adsorption properties, including key influential parameters (adsorbent dosage, pH, contact time, etc.) and adsorption mechanism, kinetics/isotherms. The results from the adsorption process conformed to pseudo-second-order kinetics (R2 = 0.998) and well fitted with the Langmuir isotherm having 191.1 mg/g maximum adsorption capacity. The adsorption mechanism of AgN/MOF-5 (1:3) was due to the interactions of π-π stacking, Ag-N-MOF covalent bonding and hydrogen bonding. Thus, AgN/MOF-5 (1:3) is a potential adsorbent for the removal of aqueous MNZ. The adsorption process is endothermic, spontaneous, and feasible based on the obtained thermodynamic parameter of ΔHO and ΔSO having 14.72 and 0.129 kJ/mol respectively.


Assuntos
Argemone , Nanopartículas Metálicas , Poluentes Químicos da Água , Antibacterianos/análise , Metronidazol/análise , Metronidazol/química , Águas Residuárias , Poluentes Químicos da Água/química , Prata/análise , Água/química , Extratos Vegetais
5.
J Environ Sci (China) ; 115: 25-36, 2022 May.
Artigo em Inglês | MEDLINE | ID: mdl-34969452

RESUMO

High efficient removal of antibiotics during nutriments recovery for biomass production poses a major technical challenge for photosynthetic microbial biofilm-based wastewater treatment since antibiotics are always co-exist with nutriments in wastewater and resist biodegradation due to their strong biotoxicity and recalcitrance. In this study, we make a first attempt to enhance metronidazole (MNZ) removal from wastewater using electrochemistry-activated binary-species photosynthetic biofilm of Rhodopseudomonas Palustris (R. Palustris) and Chlorella vulgaris (C. vulgaris) by cultivating them under different applied potentials. The results showed that application of external potentials of -0.3, 0 and 0.2 V led to 11, 33 and 26-fold acceleration in MNZ removal, respectively, as compared to that of potential free. The extent of enhancement in MNZ removal was positively correlated to the intensities of photosynthetic current produced under different externally applied potentials. The binary-species photoelectrogenic biofilm exhibited 18 and 6-fold higher MNZ removal rate than that of single-species of C. vulgaris and R. Palustris, respectively, due to the enhanced metabolic interaction between them. Application of an external potential of 0V significantly promoted the accumulation of tryptophan and tyrosine-like compounds as well as humic acid in extracellular polymeric substance, whose concentrations were 7.4, 7.1 and 2.0-fold higher than those produced at potential free, contributing to accelerated adsorption and reductive and photosensitive degradation of MNZ.


Assuntos
Chlorella vulgaris , Microalgas , Purificação da Água , Biofilmes , Matriz Extracelular de Substâncias Poliméricas , Metronidazol/análise , Águas Residuárias
6.
Ecotoxicol Environ Saf ; 204: 111066, 2020 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-32781344

RESUMO

In this study, an iron-doped metal-organic framework (MOF) Fe/ZIF-8 was synthesized from ZIF-8 at room temperature. Direct carbonization of Fe/ZIF-8 under a nitrogen atmosphere produced nanoporous nitrogen doped carbon nanoparticles decorated with Fe component (Fe/NC). The Fe/NC exhibited a large surface area (1221.185 m2 g-1) and narrow pore-size distribution (3-5 nm). The nanoporous Fe/NC components along with Nafion were used to modify a glassy carbon electrode for the electrochemical determination of chloramphenicol and metronidazole via linear sweep voltammetry. Under optimal conditions, the reduction peak currents (observed at -0.237 V and -0.071 V vs. Ag/AgCl) of these analytes increased linearly with increasing chloramphenicol and metronidazole concentrations in the range of 0.1-100 µM and 0.5-30 µM, with the detection limits estimated to be 31 nM and 165 nM, respectively. This result was attributed to the large surface area, porous structure, high nitrogen content, and as well as the electrocatalytic effect of Fe atoms embeded in the carbon support. The proposed sensor was used for chloramphenicol and metronidazole analysis in samples, providing satisfactory results.


Assuntos
Carbono/química , Cloranfenicol/análise , Técnicas Eletroquímicas/métodos , Ferro/química , Estruturas Metalorgânicas/química , Metronidazol/análise , Nitrogênio/química , Animais , Cloranfenicol/urina , Eletrodos , Humanos , Limite de Detecção , Metronidazol/urina , Leite/química , Nanoporos , Soluções Oftálmicas/química , Porosidade , Comprimidos/química
7.
Molecules ; 26(1)2020 Dec 30.
Artigo em Inglês | MEDLINE | ID: mdl-33396585

RESUMO

A suitable HPLC method has been selected and validated for rapid simultaneous separation and determination of four imidazole anti-infective drugs, secnidazole, omeprazole, albendazole, and fenbendazole, in their final dosage forms, in addition to human plasma within 5 min. The method suitability was derived from the superiority of using the environmentally benign solvent, methanol over acetonitrile as a mobile phase component in respect of safety issues and migration times. Separation of the four anti-infective drugs was performed on a Thermo Scientific® BDS Hypersil C8 column (5 µm, 2.50 × 4.60 mm) using a mobile phase consist of MeOH: 0.025 M KH2PO4 (70:30, v/v) adjusted to pH 3.20 with ortho-phosphoric acid at room temperature. The flow rate was 1.00 mL/min and maximum absorption was measured with UV detector set at 300 nm. Limits of detection were reported to be 0.41, 0.13, 0.18, and 0.15 µg/mL for secnidazole, omeprazole, albendazole, and fenbendazole, respectively, showing a high degree of the method sensitivity. The method of analysis was validated according to Food and Drug Administration (FDA)guidelines for the determination of the drugs, either in their dosage forms with highly precise recoveries, or clinically in human plasma, especially regarding pharmacokinetic and bioequivalence studies.


Assuntos
Anti-Infecciosos/química , Química Farmacêutica/métodos , Cromatografia Líquida de Alta Pressão/métodos , Imidazóis/análise , Albendazol/análise , Albendazol/sangue , Calibragem , Técnicas de Química Analítica , Formas de Dosagem , Fenbendazol/análise , Fenbendazol/sangue , Humanos , Concentração de Íons de Hidrogênio , Imidazóis/sangue , Metronidazol/análogos & derivados , Metronidazol/análise , Metronidazol/sangue , Omeprazol/análise , Omeprazol/sangue , Segurança do Paciente , Reprodutibilidade dos Testes , Solventes , Temperatura , Raios Ultravioleta , Estados Unidos , United States Food and Drug Administration
8.
Mikrochim Acta ; 186(9): 652, 2019 08 28.
Artigo em Inglês | MEDLINE | ID: mdl-31463802

RESUMO

Non-conjugated polymer carbon dots (PCDs) with a 9% fluorescence quantum yield were synthesized by a pyrolytic method using polyethyleneimine as the sole precursor. The PCDs have an average size about 2.1 nm and a blue fluorescence, with excitation/emission maxima at 380/457 nm, that is quenched by the drug metronidazole. The method has a linear response in the 0.06-15 µg mL-1 metronidazole concentration range and a 20 ng mL-1 detection limit. Milk samples were spiked at two levels (0.6 and 5.0 µg mL-1), and the recoveries of metronidazole are in the range of 96.7-102.2%. Graphical abstract Schematic representation of preparation of non-conjugated polymer carbon dots (PCDs) and detection of metronidazole. Metronidazole with negative charge is easy to produce electrostatic interaction with polyethyleneimine chain with positive charge, which leads to PCDs fluorescence quenching, so as to realize metronidazole detection.


Assuntos
Carbono/química , Fluorometria/métodos , Metronidazol/análise , Polímeros/química , Pontos Quânticos/química , Animais , Limite de Detecção , Metronidazol/química , Leite/química
9.
Luminescence ; 33(4): 704-712, 2018 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-29520942

RESUMO

In this work, carbon dots (CDs) with a high quantum yield (22.3%) were easily prepared by hydrothermal pyrolysis of acid fuchsin 6B and hydrogen peroxide at 180°C for 10 h. The resultant CDs possess a narrow size distribution in the range of 2.6 to 3.2 nm and emit blue fluorescence. Interestingly, the absorption band of metronidazole (MTZ) centered at 318 nm can complementary overlap with the excitation band of the as-prepared CDs centered at 320 nm, resulting in an inner filter effect (IFE) in high efficiency. In fact, the fluorescence quenching of the CDs depends on the concentration of MTZ. Therefore, a simple method for the detection of MTZ can be established using the CDs-based sensor via the IFE. The linear range of the proposed method was 0-10 µg mL-1 with the limit of detection as low as 0.257 µg mL-1 . This CDs-based sensor had been applied for the detection of MTZ in honey and MTZ tablets with the recoveries in the range of 98.0% to 105.1% and 95.7% to 106.5%, respectively. Therefore, the as-prepared CDs have a potential to be developed as a MTZ sensor with high selectivity, sensitivity and accuracy.


Assuntos
Carbono/química , Corantes Fluorescentes/química , Mel/análise , Metronidazol/análise , Pontos Quânticos/química , Concentração de Íons de Hidrogênio , Tamanho da Partícula , Cloreto de Sódio/química , Comprimidos/química , Temperatura
10.
Bull Environ Contam Toxicol ; 100(3): 395-401, 2018 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-29299634

RESUMO

A molecularly imprinted polymer was developed and evaluated for selective determination of metronidazole (MNZ) in wastewater. This was achieved by using sodium methacrylate as monomer, toluene as porogen, ethylene glycol dimethacrylate as crosslinker, azobisisobutyronitrile as initiator and metronidazole as template molecule to generate the selectivity of the polymer for the compound, as well as non-imprinted polymers were synthesized. Two different polymerization approaches were used, bulk and emulsion and the polymers obtained by emulsion presented higher retention percentages the MIP 2-M presented the higher retention (83%). The performed method, was validated in fortified water, showing linearity from 10 up to 1000 ng/mL; limit of detection and quantification for compound were between 3 and 10 ng/mL, respectively. Finally, the method was applied in samples of a wastewater treatment plant in the city of San Luis Potosí, México, and the concentrations of MNZ in these samples were 84.1-114 ng/mL.


Assuntos
Metronidazol/análise , Impressão Molecular/métodos , Ácidos Polimetacrílicos/síntese química , Águas Residuárias/química , Poluentes Químicos da Água/análise , Adsorção , Limite de Detecção , Metacrilatos/química , México , Nitrilas/química , Ácidos Polimetacrílicos/química , Propriedades de Superfície , Tolueno/química
11.
Pak J Pharm Sci ; 31(5): 1903-1910, 2018 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-30150187

RESUMO

The current study was designed to evaluate mucoadhesive buccal tablet containing metronidazole (MTZ) for local action aided by Hydroxypropylmethylcellulose K4M (HPMC) and Carbopol 940® (CP) as mucoadhesive polymers with other ingredients like sodium starch glycolate (SSG), polyvinyl pyrollidone K30 (PVP) as disintegrant and binders respectively. Formulations (F1-F8) were prepared by direct compression method and characterized for different physicochemical parameters. Results showed that the average weight and friability were within USP limits. Maximum mucoadhesive time was observed for F2 (14 hr) containing moderate amount of HPMC and CP used in the study. Up most mucoadhesive strength value was observed with F3 containing highest amount of HPMC used. Results indicated that high amount of HPMC was linked with the moderate to higher mucoadhesive strength and time. Maximum swelling index was observed in F7 (191.3%). Only F1-F3 showed complete in vitro MTZ release within 3 hr. Formulations containing PVP released MTZ incompletely over time while SSG released earlier. Formulation F1 was considered best in terms of MTZ release (100.5%) with diffusion based Korsmeyer-Peppas release kinetics. Therefore, MTZ exhibiting best physicochemical characters in mucoadhesive buccal tablet was found in F1 containing HPMC and CP in amounts of 37.5 mg and 25 mg, respectively, for local action.


Assuntos
Anti-Infecciosos/química , Desenvolvimento de Medicamentos/métodos , Gengivite , Metronidazol/química , Mucosa Bucal , Periodontite , Adesividade , Anti-Infecciosos/administração & dosagem , Anti-Infecciosos/análise , Gengivite/tratamento farmacológico , Gengivite/microbiologia , Humanos , Derivados da Hipromelose/administração & dosagem , Derivados da Hipromelose/análise , Derivados da Hipromelose/química , Metronidazol/administração & dosagem , Metronidazol/análise , Mucosa Bucal/efeitos dos fármacos , Mucosa Bucal/microbiologia , Periodontite/tratamento farmacológico , Periodontite/microbiologia , Comprimidos
12.
Artigo em Inglês | MEDLINE | ID: mdl-28920773

RESUMO

Metronidazole (MNZ) removal by two adsorbents, i.e., concrete-containing graphene (CG) and powder-activated carbon (PAC), was investigated via batch-mode experiments and the outcomes were used to analyze the kinetics, equilibrium and thermodynamics of MNZ adsorption. MNZ sorption on CG and PAC has followed the pseudo-second-order kinetic model, and the thermodynamic parameters revealed that MNZ adsorption was spontaneous on PAC and non-spontaneous on CG. Subsequently, two-parameter isotherm models, i.e., Langmuir, Freundlich, Temkin, Dubinin-Radushkevich and Elovich models, were applied to evaluate the MNZ adsorption capacity. The maximum MNZ adsorption capacities ([Formula: see text]) of PAC and CG were found to be between 25.5-32.8 mg/g and 0.41-0.002 mg/g, respectively. Subsequently, the effects of pH, temperature and adsorbent dosage on MNZ adsorption were evaluated by a central composite design (CCD) approach. The CCD experiments have pointed out the complete removal of MNZ at a much lower PAC dosage by increasing the system temperature (i.e., from 20°C to 40°C). On the other hand, a desorption experiment has shown 3.5% and 1.7% MNZ removal from the surface of PAC and CG, respectively, which was insignificant compared to the sorbed MNZ on the surface by adsorption. The overall findings indicate that PAC and CG with higher graphene content could be useful in MNZ removal from aqueous systems.


Assuntos
Carvão Vegetal/química , Materiais de Construção , Grafite/química , Metronidazol/análise , Poluentes Químicos da Água/análise , Purificação da Água/métodos , Adsorção , Concentração de Íons de Hidrogênio , Cinética , Metronidazol/química , Modelos Teóricos , Pós , Projetos de Pesquisa , Termodinâmica , Poluentes Químicos da Água/química
13.
J Environ Manage ; 169: 116-25, 2016 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-26731310

RESUMO

This study analyzed the overall adsorption rate of metronidazole, dimetridazole, and diatrizoate on activated carbons prepared from coffee residues and almond shells. It was also elucidated whether the overall adsorption rate was controlled by reaction on the adsorbent surface or by intraparticle diffusion. Experimental data of the pollutant concentration decay curves as a function of contact time were interpreted by kinetics (first- and second-order) and diffusion models, considering external mass transfer, surface and/or pore volume diffusion, and adsorption on an active site. The experimental data were better interpreted by a first-order than second-order kinetic model, and the first-order adsorption rate constant varied linearly with respect to the surface area and total pore volume of the adsorbents. According to the diffusion model, the overall adsorption rate is governed by intraparticle diffusion, and surface diffusion is the main mechanism controlling the intraparticle diffusion, representing >90% of total intraparticle diffusion.


Assuntos
Café , Diatrizoato/química , Dimetridazol/química , Metronidazol/química , Prunus dulcis/química , Purificação da Água/métodos , Adsorção , Carvão Vegetal/química , Diatrizoato/análise , Difusão , Cinética , Metronidazol/análise
14.
Anal Bioanal Chem ; 407(13): 3875-80, 2015 May.
Artigo em Inglês | MEDLINE | ID: mdl-25749799

RESUMO

In this study, novel magnetic molecularly imprinted polymers (MMIPs) were developed as a sorbent for solid-phase extraction (SPE) and used for the selective separation of metronidazole (MNZ) in cosmetics; MNZ was detected by high-performance liquid chromatography (HPLC). First, magnetic Fe3O4 nanoparticles (NPs) were prepared by the co-precipitation of Fe(2+)and Fe(3+) ions in an ammonia solution; then oleic acid (OA) was modified onto the surface of Fe3O4NPs. Finally, the MMIP was prepared by aqueous suspension polymerization, involving the copolymerization of Fe3O4NPs@OA with MNZ as the template molecule, methacrylic acid (MAA) as the functional monomer, ethylene glycol maleic rosinate acrylate (EGMRA) as the cross-linking agent, and 2,2-azobisisobutyronitrile (AIBN) as the initiator. The MMIP materials showed high selective adsorption capacity and fast binding kinetics for MNZ; the maximum adsorption amount of the MMIP to MNZ was 46.7 mg/g. The assay showed a linear range from 0.1 to 20.0 µg/mL for MNZ with the correlation coefficient 0.999. The relative standard deviations (RSD) of intra- and inter-day ranging from 0.71 to 2.45% and from 1.06 to 5.20% were obtained. The MMIP can be applied to the enrichment and determination of MNZ in cosmetic products with the recoveries of spiked toner, powder, and cream cosmetic samples ranging from 90.6 to 104.2, 84.1 to 91.4, and 90.3 to 100.4%, respectively, and the RSD was <3.54%.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Cosméticos/análise , Nanopartículas de Magnetita/química , Metronidazol/análise , Metronidazol/química , Impressão Molecular/métodos , Cosméticos/química , Contaminação de Medicamentos/prevenção & controle , Nanopartículas de Magnetita/ultraestrutura , Polímeros/química
15.
Ann Pharm Fr ; 73(5): 351-60, 2015 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-26024556

RESUMO

This work deals with the development, validation and application of an HPLC-DAD method for the determination of a ternary mixture containing amoxicillin (AX), metronidazole (MZ) and the proton pump inhibitor rabeprazole sodium (RB). This triple therapy is used for treatment of Helicobacter pylori infection. Effective chromatographic separation between the three drugs was achieved using Thermo Hypersil BDS-C8 (4.6×250mm, 5µm particle size) column and a mobile phase composed of phosphate buffer pH 7 and acetonitrile (70: 30, by volume). The mobile phase was pumped isocratically at a flow rate of 1 mL/min. Quantification of the analytes was based on measuring their peak areas at 230nm for both AX and RB, and at 319nm for MZ. AX, MZ and RB eluted at retention times 2.36, 3.55 and 8.72min respectively. The reliability and analytical performance of the proposed HPLC procedure were statistically validated with respect to linearity, ranges, precision, accuracy, selectivity, robustness, detection and quantification limits. The linear dynamic ranges were 25-250, 25-250 and 5-50µg/mL for AX, MZ and RB respectively with correlation coefficients>0.9998. The validated method was successfully applied to the analysis of several laboratory-prepared mixtures as well as simulated intestinal fluid samples spiked with the three drugs.


Assuntos
Amoxicilina/análise , Antibacterianos/análise , Líquidos Corporais/química , Metronidazol/análise , Inibidores da Bomba de Prótons/análise , Rabeprazol/análise , Calibragem , Cromatografia Líquida de Alta Pressão , Estabilidade de Medicamentos , Humanos , Reprodutibilidade dos Testes
16.
AAPS PharmSciTech ; 15(5): 1070-5, 2014 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-24848759

RESUMO

Biowaivers for class I drugs according to the biopharmaceutics classification system (BCS) were first introduced in 2000. The in vitro equivalence can be used to document bioequivalence between products. This study compared the in vitro dissolution behavior of two BCS class I drugs, amoxicillin and metronidazole, which are sold in China. Identifying a reference product on the Chinese domestic market was impossible. Three 250-mg and two 500-mg amoxicillin capsules and four metronidazole tablet products were tested. None of the amoxicillin products and three of the four metronidazole tablets were found to be equivalent to each other when the same strengths were compared. The bioequivalence of products that fail the in vitro test can be established via in vivo clinical studies which are expensive and time consuming. Establishing nationally or globally accepted reference products may provide regulatory agencies with an efficient mechanism approving high quality generics.


Assuntos
Medicamentos Genéricos/normas , Algoritmos , Amoxicilina/análise , Amoxicilina/normas , Cápsulas/análise , Química Farmacêutica , China , Cromatografia Líquida de Alta Pressão , Medicamentos Genéricos/análise , Metronidazol/análise , Metronidazol/normas , Solubilidade , Comprimidos/análise
17.
Zhonghua Wai Ke Za Zhi ; 52(10): 775-80, 2014 Oct.
Artigo em Zh | MEDLINE | ID: mdl-25573219

RESUMO

OBJECTIVE: To study the concentrations and pharmacokinetics of 6 different kinds of antibiotics in rabbit bile, and evaluate their microbicidal potential. METHODS: Thirty-six health rabbits were randomly divided into 6 groups, and each group was 6 rabbits. After anaesthesia, the common bile duct of rabbit was isolated and cumulated with a silicone tube. The rabbits were administered intravenously with the equal-effect dose of antibiotics. Bile (1.5 ml) was collected at different time points after administration, and the concentration of antibiotics of bile was assayed by high performance liquid chromatography. The bile drug concentration-time data were processed by software to figure out the pharmacokinetic parameters such as maximum concentration (C(max)), peak time (T(max)), half-life time (T(1/2)), clearance (CL) and apparent volume of distribution (VD). The bile antibiotics concentration contrasted to the minimum inhibitory concentration (MIC), and attained the bactericidal index (C(max)/MIC) and the time when the drug concentration exceeded the MIC (T(>MIC)). RESULTS: The C(max) and T1/2 of each antibiotic were as the followings: piperacillin (7 950 ± 3 023) mg/L and (1.97 ± 1.23) h, ceftriaxone (1 104 ± 248) mg/L and (3.14 ± 0.57) h, cefoperazone (5 215 ± 2 225) mg/L and (0.89 ± 0.13) h, meropenem (31.97 ± 12.44) mg/L and (0.36 ± 0.11) h, levofloxacin (66.3 ± 36.9) mg/L and (3.32 ± 2.57) h, metronidazole (28.2 ± 10.2) mg/L and (0.81 ± 0.33) h, respectively. Piperacillin/tazobactam and cefoperazone/sulbactam had the largest bactericidal index and the longest T(>MIC), and their bactericidal indexes were (62.1 ± 23.6) - (993.8 ± 377.9) and (164.8 ± 69.0) - (659.3 ± 275.9), their T(>MIC) were (6.00 ± 2.53) - (8.00 ± 0.00) h and (6.33 ± 1.97) - (8.00 ± 0.00) h. The bactericidal index and T(>MIC) of levofloxacin were the smallest, which were (2.1 ± 1.2) - (8.3 ± 4.6) and (0.54 ± 0.25) - (2.67 ± 1.03) h . Ceftriaxone and meropenem were as the medium, and their bactericidal indexes and T(>MIC) were (4.3 ± 1.0) - (69.2 ± 15.5) , (1.42 ± 0.65) - (8.00 ± 0.00) h and (2.0 ± 0.8) - (1 031.3 ± 401.4) , (0.29 ± 0.10) - (1.83 ± 0.26) h. The bactericidal index of metronidazole to anaerobic ranged from 7.4 to 294.9, and the T(>MIC) ranged from 1.88 to 5.00 h. CONCLUSIONS: The bile concentrations of six antibiotics all exceed their effective bactericidal concentrations. The concentration-time curves of piperacillin, cefoperazone, meropenem and metronidazole conformed to one-compartment model, and ceftriaxone and levofloxacin are conformed to two-compartment model. Piperacillin/tazobactam and cefoperazone/sulbactam have the largest bactericidal index and the longest T(>MIC), so they can be chosen as the first choice for the therapy of hepatobiliary infection.For the anaerobic, the microbicidal potential of metronidazole is high.


Assuntos
Antibacterianos/análise , Antibacterianos/farmacocinética , Bile/química , Bile/efeitos dos fármacos , Animais , Cefoperazona/análise , Cefoperazona/farmacocinética , Combinação de Medicamentos , Meropeném , Metronidazol/análise , Metronidazol/farmacocinética , Testes de Sensibilidade Microbiana , Ácido Penicilânico/análogos & derivados , Ácido Penicilânico/análise , Ácido Penicilânico/farmacocinética , Piperacilina/análise , Piperacilina/farmacocinética , Combinação Piperacilina e Tazobactam , Coelhos , Distribuição Aleatória , Sulbactam/análise , Sulbactam/farmacocinética , Tienamicinas/análise , Tienamicinas/farmacocinética
18.
Chemosphere ; 351: 141219, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38224750

RESUMO

Degradation of antibiotics through electrocatalytic oxidation has recently been comprehended as a promising strategy in wastewater treatment. Herein, nitrogen and sulphur doped graphene oxide (N,S-rGO) nanosheets were synthesized and employed as metal-free anodic material for electrochemical degradation of antibiotics, viz. metronidazole (MNZ) and tetracycline (TC). The synthesized anodic material was characterized using various spectral techniques and further the electrochemical behaviour of N,S-rGO was thoroughly examined. Thereafter, the N,S-rGO material was then employed as the anode material towards the electrocatalytic degradation of antibiotics. Parameters such as initial concentration of the antibiotics and current densities were varied and their effect towards the degradation of MNZ and TC were probed. Notably, the N,S-rGO based anode has shown impressive removal efficiency of 99% and 98.5%, after 120 min of reaction time for MNZ and TC, respectively, under optimized conditions. The obtained results including the kinetic parameters, removal efficiency and electrical efficiency ensure that the prepared anodic material has huge prospective towards real-time application for removal of antibiotics from water.


Assuntos
Metronidazol , Águas Residuárias , Metronidazol/análise , Carbono , Estudos Prospectivos , Antibacterianos/química , Tetraciclina/química , Metais , Eletrodos
19.
Chemosphere ; 359: 142279, 2024 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-38723687

RESUMO

The widespread use and misuse of antibiotics in pharmaceuticals and animal farming has resulted in their accumulation in food sources and the environment, posing significant threats to human health, the environment, and the global economy. In this study, we have developed a hypersensitive, and ultra-selective electrochemical sensor, the first of its kind, by integrating a thermally annealed gold-silver alloy nanoporous matrix (TA-Au-Ag-ANpM) with reduced graphene oxide (r-GO) and poly(glycine) at the surface of a glassy carbon electrode (GCE). This sensor aims to detect life-threatening metronidazole (MTZ) residues in food samples. TA-Au-Ag-ANpM/r-GO/poly(glycine)/GCE was thoroughly characterized using a range of analytical techniques, including UV-Vis, FT-IR, XRD, SEM, and EDX. Furthermore, its electrochemical properties were investigated by cyclic voltammetry (CV), square wave voltammetry (SWV), and electrochemical impedance spectroscopy (EIS). The sensor exhibited outstanding performance, with a broad linear range of 2.0 pM-410 µM. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.0312 pM and 0.104 pM, respectively. The TA-Au-Ag-ANpM/r-GO/poly(glycine)/GCE exhibited exceptional reproducibility, repeatability, stability, and resistance to interferences. Moreover, the sensor demonstrated outstanding performance in detecting MTZ residues in milk powder, pork, and chicken meat samples, achieving very good recoveries (96.9%-101.4%) with a relative standard deviation (RSD) below 5%. This performance highlights the potential for practical applications in food safety and quality monitoring. Therefore, the developed sensor contributes to the advancement of electrochemical sensing technology and its application in ensuring food safety and integrity by combating antibiotic residues.


Assuntos
Técnicas Eletroquímicas , Contaminação de Alimentos , Grafite , Limite de Detecção , Metronidazol , Metronidazol/análise , Grafite/química , Técnicas Eletroquímicas/métodos , Contaminação de Alimentos/análise , Animais , Eletrodos , Ouro/química , Análise de Alimentos/métodos , Prata/química , Reprodutibilidade dos Testes , Antibacterianos/análise , Resíduos de Drogas/análise
20.
J Fluoresc ; 23(3): 599-604, 2013 May.
Artigo em Inglês | MEDLINE | ID: mdl-23471624

RESUMO

In the present paper, we report the fabrication of a new sensing membrane for fluorescence detection of metronidazole (MNZ). Briefly, a pyrenebutyric acid derivative, 2-(methacryloyloxy) ethyl-4-(1-pyrenyl) butanoate (MPB) with a double bond, was synthesized and copolymerized with 2-hydroxyethylmethacrylate (HEMA) on the activated glass surface by thermal initiation in the presence of cross-linker. The sensor responds linearly to metronidazole in the concentration range of 1.23~35.48 mg.L(-1) in aqueous solution with a detection limit of 0.36 mg.L(-1). The lifetime is enhanced by covalently immobilizing the pyrenebutyric acid derivative on glass slide, which hinders leaching of the dye from the membrane. The sensor could be regenerated after use by washing in methanol (RSD = 2.42 %), and it shows sufficient stability, and selectivity. Interference of other pharmaceuticals on membrane performance is discussed. The developed membrane has been successfully applied for the direct determination of metronidazole in human serum sample without pretreatment.


Assuntos
Técnicas de Química Analítica/instrumentação , Corantes Fluorescentes/química , Membranas Artificiais , Metronidazol/análise , Pirenos/química , Soluções Tampão , Ácido Butírico/química , Humanos , Concentração de Íons de Hidrogênio , Metronidazol/sangue , Metronidazol/química , Reprodutibilidade dos Testes , Espectrometria de Fluorescência
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