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1.
Int J Biol Macromol ; 267(Pt 1): 131321, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38570001

RESUMO

The improper usage of levofloxacin (LEV) endangers both environmental safety and human public health. Therefore, trace analysis and detection of LEV have extraordinary significance. In this paper, a novel molecularly imprinted polymer (MIP) electrochemical sensor was developed for the specific determination of LEV by electrochemical polymerization of o-phenylenediamine (o-PD) using poly(3,4-ethylenedioxythiophene)/chitosan (PEDOT/CS) with a porous structure and rich functional groups as a carrier and LEV as a template molecule. The morphology, structure and properties of the modified materials were analyzed and studied. The result showed that the electron transfer rate and the electroactive strength of the electrode surface are greatly improved by the interconnection of PEDOT and CS. Meanwhile, PEDOT/CS was assembled by imprinting with o-PD through non-covalent bonding, which offered more specific recognition sites and a larger surface area for the detection of LEV and effectively attracted LEV through intermolecular association. Under the optimized conditions, MIP/PEDOT/CS/GCE showed good detection performance for LEV in a wide linear range of 0.0019- 1000 µM, with a limit of detection (LOD, S/N = 3) of 0.4 nM. Furthermore, the sensor has good stability and selectivity, and exhibits excellent capabilities in the microanalysis of various real samples.


Assuntos
Compostos Bicíclicos Heterocíclicos com Pontes , Quitosana , Técnicas Eletroquímicas , Levofloxacino , Impressão Molecular , Polímeros Molecularmente Impressos , Polímeros , Quitosana/química , Levofloxacino/análise , Levofloxacino/química , Polímeros/química , Compostos Bicíclicos Heterocíclicos com Pontes/química , Impressão Molecular/métodos , Técnicas Eletroquímicas/métodos , Polímeros Molecularmente Impressos/química , Eletrodos , Limite de Detecção , Humanos
2.
Inorg Chem ; 63(18): 8336-8341, 2024 May 06.
Artigo em Inglês | MEDLINE | ID: mdl-38651971

RESUMO

A cube-like Zn(II)-Eu(III) nanocluster 1 (molecular sizes: 1.8 × 2.0 × 2.0 nm) was constructed by the use of a new long-chain Schiff base ligand. It shows a ratiometric fluorescence response to levofloxacin (LFX) with high sensitivity and selectivity, which can be expressed as I615 nm/I550 nm = A*[LFX]2 + B*[LFX] + C. It is used to quantitatively detect the LFX concentrations in fetal calf serum (FCS) and tablets sold in pharmacy. Filter paper strips bearing 1 can be used to qualitatively detect LFX by a color change to red under a UV lamp. 1 and its hybrid with sodium alginate (SA), 1@SA, display potential applications in the qualitative detection of LFX in FCS and the medicine. The limit of detection of 1 to LFX is as low as 2.1 × 10-2 nM.


Assuntos
Alginatos , Európio , Levofloxacino , Zinco , Alginatos/química , Zinco/química , Zinco/sangue , Levofloxacino/sangue , Levofloxacino/análise , Európio/química , Espectrometria de Fluorescência , Animais , Humanos , Bovinos , Comprimidos , Corantes Fluorescentes/química
3.
Huan Jing Ke Xue ; 45(3): 1468-1479, 2024 Mar 08.
Artigo em Chinês | MEDLINE | ID: mdl-38471862

RESUMO

Pharmaceuticals and personal care products (PPCPs) are a group of emerging contaminants causing detrimental effects on aquatic living organisms even at low doses. To investigate the contamination characteristics and ecological risks of PPCPs in drains flowing into the Yellow River of Ningxia, 21 PPCPs were detected and analyzed using solid phase extraction and ultra-high performance liquid chromatography-mass spectrometry in this study. All 21 targeted compounds were detected in the drains, with total concentrations ranging from 47.52 to 1 700.96 ng·L-1. Ciprofloxacin, acetaminophen, benzophenone-3, and diethyltoluamide were the more commonly detected compounds, with detection frequencies exceeding 80%. The five highest-concentration PPCPs were acetaminophen, diethyltoluamide, caffeine, benzophenone-3, and levofloxacin, with the maximum concentrations of 597.21, 563.23, 559.00, 477.28, and 473.07 ng·L-1, respectively. Spatial analysis showed that the pollution levels of PPCPs in the drains of the four cities were different, with average concentrations of ∑PPCPs in the order of Yinchuan>Shizuishan>Wuzhong>Zhongwei. The total concentration of PPCPs before flowing into the Yellow River ranged from 124.82 to 1 046.61 ng·L-1. Source analysis showed that livestock and poultry breeding wastewater was the primary source for sulfadiazine and oxytetracycline, whereas medical wastewater was the primary source for levofloxacin and ciprofloxacin. The primary sources of triclocarban and triclosan were domestic sewage and industrial wastewater, whereas the primary source of caffeine and diethyltoluamide was domestic sewage. The pollution of diciofenac, cimetidine, triclocarban, and triclosan in the drains was positively correlated with the regional population and economic development level. The ecological risk assessment indicated that levofloxacin, diclofenac, gemfibrozil, benzophenone-3, and triclocarban posed high risks to aquatic organisms in drains flowing into the Yellow River. It is worthwhile to consider the mixture risk of the PPCPs that exhibited high risk at most sampling sites.


Assuntos
Benzofenonas , Carbanilidas , Cosméticos , Triclosan , Poluentes Químicos da Água , Acetaminofen , Organismos Aquáticos , Cafeína/análise , Ciprofloxacina , Cosméticos/análise , Monitoramento Ambiental/métodos , Levofloxacino/análise , Preparações Farmacêuticas , Medição de Risco , Rios/química , Esgotos/análise , Águas Residuárias , Poluentes Químicos da Água/análise
4.
Chemosphere ; 355: 141763, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38522672

RESUMO

The fluoroquinolones ciprofloxacin, danofloxacin, enoxacin, levofloxacin and lomefloxacin, occur in water bodies worldwide and therefore pose a threat to the aquatic environment. Advanced purification procedures, such as electrochemical oxidation, may act as a remedy since they contribute to eliminating contaminants and prevent micropollutants from entering open water bodies. By electrochemical treatment in a micro-flow reactor equipped with a boron-doped diamond (BDD) electrode, the fluoroquinolones were efficiently degraded. A total of 15 new products were identified using high-performance high-resolution chromatography coupled with high-resolution multifragmentation mass spectrometry. The ecotoxicity of the emerging transformation products was estimated through in silico quantitative structure activity relationship analysis. Almost all transformation products were predicted less ecotoxic than the initial compounds. The fluoroquinolone degradation followed three major mechanisms depending on the voltage during the electrochemical oxidation. At approximately 1 V, the reactions started with the elimination of molecular hydrogen from the piperazine moiety. At approx. 1.25 V, methyl and methylene groups were eliminated. At 1.5 V, hydroxyl radicals, generated at the BDD electrode, led to substitution at the piperazine ring. This novel finding of the three reactions depending on voltage contributes to the mechanistic understanding of electrochemical oxidation as potential remedy against fluoroquinolones in the aquatic environment.


Assuntos
Ciprofloxacina , Poluentes Químicos da Água , Ciprofloxacina/química , Levofloxacino/análise , Enoxacino/análise , Diamante/química , Fluoroquinolonas/análise , Piperazina , Oxirredução , Eletrodos , Água , Poluentes Químicos da Água/análise
5.
J Environ Manage ; 354: 120329, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38373375

RESUMO

Microplastics (MPs) usually appear in the aquatic environment as complex pollutants in combination with other environmental pollutants, such as levofloxacin (LVFX). After a 45-day exposure to LVFX and MPs with different particle sizes at environmental levels, LVFX was neurotoxic to Rana nigromaculata tadpoles. The order of the effects of the exposure treatment on tadpole behavior was: LVFX-MP3>LVFX-MP1>LVFX-MP2 ≥ LVFX. Results of transcriptome analysis of tadpole brain tissue showed that LVFX in combination with 0.10 and 10.00 µm MP interferes with the nervous system through the cell adhesion molecules pathway. Interestingly, the order of effects of the co-exposure on oxidative stress in the intestine was inconsistent with that of tadpole behavior. We found that Paraacteroides might be a microplastic indicator species for the gut microbiota of aquatic organisms. The results of the targeted metabolism of neurotransmitters in the intestine suggest that in the LVFX-MP2 treatment, LVFX alleviated the intestinal microbiota disorder caused by 1.00 µm MP, by regulating intestinal microbiota participating in the TCA cycle VI and gluconeogenesis and tetrapyrrole biosynthesis I, while downregulating Met and Orn, and upregulating 5HIAA, thereby easing the neurotoxicity to tadpoles exposed to LVFX-MP2. This work is of great significance for the comprehensive assessment of the aquatic ecological risks of microplastics-antibiotic compound pollutants.


Assuntos
Poluentes Ambientais , Poluentes Químicos da Água , Animais , Levofloxacino/análise , Microplásticos/toxicidade , Plásticos , Tamanho da Partícula , Intestinos/química , Encéfalo , Ranidae , Poluentes Ambientais/análise , Poluentes Químicos da Água/toxicidade , Poluentes Químicos da Água/análise
6.
J Environ Manage ; 344: 118718, 2023 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-37541001

RESUMO

Antibiotic-containing wastewater is a typical biochemical refractory organic wastewater and general treatment methods cannot effectively and quickly degrade the antibiotic molecules. In this study, a novel boron-doped diamond (BDD) pulse electrochemical oxidation (PEO) technology was proposed for the efficient removal of levofloxacin (LFXN) from wastewater. The effects of current density (j), initial pH (pH0), frequency (f), electrolyte types and initial concentration (c0(LFXN)) on the degradation of LFXN were systematically investigated. The degradation kinetics under four different processes have also been studied. The possible degradation mechanism of LFXN was proposed by Density functional theory calculation and analysis of degradation intermediates. The results showed that under the optimal parameters, the COD removal efficiency (η(COD)) was 94.4% and the energy consumption (EEC) was 81.43 kWh·m-3 at t = 120 min. The degradation of LFXN at pH = 2.8/c(H2O2) followed pseudo-first-order kinetics. The apparent rate constant was 1.33 × 10-2 min-1, which was much higher than other processes. The degradation rate of LFXN was as follows: pH = 2.8/c(H2O2) > pH = 2.8 > pH = 7/c(H2O2) > pH = 7. Ten aromatic intermediates were formed during the degradation of LFXN, which were further degraded to F-, NH4+, NO3-, CO2 and H2O. This study provides a promising approach for efficiently treating LFXN antibiotic wastewater by pulsed electrochemical oxidation with a BDD electrode without adding H2O2.


Assuntos
Águas Residuárias , Poluentes Químicos da Água , Antibacterianos , Levofloxacino/análise , Peróxido de Hidrogênio , Poluentes Químicos da Água/química , Boro/química , Diamante/química , Oxirredução , Eletrodos
7.
Sci Total Environ ; 862: 160773, 2023 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-36509275

RESUMO

Levofloxacin (LEV) is prone to be retained in aquifers due to its strong adsorption affinity onto sand, thus posing a threat to groundwater quality. In-situ injection technology for remediating LEV-contaminated soil and groundwater is still challenging owing to the lack of appropriate remedial agents. Herein, two novel multi-component porous covalent-organic polymers (namely, SLEL-1 and SLEL-2) with alkyl chains were constructed through Schiff-base reactions to adsorb LEV from an aqueous solution, in which the kinetics, isotherms, influenced factors were investigated. Plausible adsorption mechanisms were proposed through characterization and experimental analysis, including pore filling effect, π-π electron-donor-acceptor (EDA) interaction, hydrogen bonding force, hydrophobic-hydrophobic interaction as well as electrostatic force. In addition, response surface methodology (RSM) revealed the treatment optimization and reciprocal relationship within multi-variables. Furthermore, taking advantage of favorable dispersion and outstanding competitive behavior, SLEL-1 was established as an in-situ adsorptive agent in dynamic saturated columns on a laboratory scale to investigate the removal of LEV from water-bearing stratum. Overall, the findings of this work provided an insight into the fabrication of SLELs as long-term mobile and reusable adsorptive agents for practical in-situ applications in the future.


Assuntos
Levofloxacino , Poluentes Químicos da Água , Levofloxacino/análise , Areia , Porosidade , Polímeros , Adsorção , Poluentes Químicos da Água/química
8.
Bioresour Technol ; 351: 127025, 2022 May.
Artigo em Inglês | MEDLINE | ID: mdl-35307521

RESUMO

This study evaluated the relationship between pyrolysis temperature (300-900 ℃), characteristics of swine manure (SM)-derived biochar (BC), and its adsorption of levofloxacin (LEV). The surface structure and chemistry of SM-derived BCs were characterized using Brunauer-Emmett-Teller analysis, scanning electron microscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, Raman spectroscopy, and X-ray photoelectron spectroscopy. According to the characteristic analysis, the surface area and graphitization degree of SM-derived BC increased as temperature rose. The highest adsorption capacity was achieved by BC-900 (158 mg/g); this level was higher than that achieved in previous studies and comparable to that of commercial activated carbons. Characterization and adsorption experiments indicated that pore-filling, π-π stacking interaction, π-π electron donor-acceptor, H-bonding, and hydrophobic interactions each played a critical role in the adsorption of LEV on SM-derived BC. Collectively, this study confirms the potential utility of SM-derived BC for the removal of antibiotics.


Assuntos
Levofloxacino , Poluentes Químicos da Água , Adsorção , Animais , Carvão Vegetal/química , Cinética , Levofloxacino/análise , Esterco , Espectroscopia de Infravermelho com Transformada de Fourier , Suínos , Poluentes Químicos da Água/química
9.
Artigo em Inglês | MEDLINE | ID: mdl-34801729

RESUMO

Aeromonas hydrophila is an opportunistic bacteria with an overwhelming impact on fish farming industry especially with upraising of drug resistant mutants. This study aimed to evaluate and compare the therapeutic and side effects of levofloxacin (LEV), chitosan-nanoparticles (CNPs), and fructooligosaccharides (FOS) in control of this infection in tilapia. A total of 160 Nile-tilapia divided into 8-groups; G1: negative-control, G2: infected-control, G3: non-infected-(levofloxacin (LEV) 10 mg/kg bwt), G4: non-infected-(chitosan-nanoparticles (CNPs) 1 g/kg ration), G5: non-infected-(fructooligosaccharides (FOS) 20 g/kg ration), G6: infected-LEV, G7: infected-CNPs and G8: infected-FOS for 7 days. MICs were (0.125 µg/ml and 1.25 mg/ml) for LEV and CNPs respectively. No mortalities or significant adverse effects were recorded in non-infected treated-groups while infected were (20%) LEV, (30%) CNPs, (40%) FOS and (70%) G2. Aspartate aminotransferase (AST), alanine aminotransferase (ALT) and alkaline phosphatase (ALP) decreased by LEV and CNPs than FOS while all increased total protein (TP) and albumin than G2. Malondialdehyde (MDA) significantly decreased and superoxide dismutase (SOD) and reduced glutathione (GSH) increased in all infected-treated groups than G2 in various degrees. Urea and creatinine descending order were FOS, LEV then CNPs decreased significantly than G2. LEV musculature residues, using HPLC, decreased gradually till the 5th day; 621.00 ± 0.66, 270.00 ± 0.48 then 64.00 ± 0.40, and 471.00 ± 0.79, 175.00 ± 0.52 ppb then not detected at 1st, 3rd, and 5th days of withdrawal in non-infected and infected groups respectively. Finally, LEV and CNPs were superior as bactericidal, decreasing mortalities and enzyme activities while CNPs and FOS increased performance, non-specific immunity, and antioxidant biomarkers.


Assuntos
Aeromonas hydrophila/efeitos dos fármacos , Antibacterianos/farmacologia , Doenças dos Peixes/tratamento farmacológico , Infecções por Bactérias Gram-Negativas/tratamento farmacológico , Nanopartículas/química , Ração Animal , Animais , Antibacterianos/análise , Antioxidantes/metabolismo , Aquicultura , Quitosana/química , Quitosana/farmacologia , Ciclídeos/crescimento & desenvolvimento , Ciclídeos/microbiologia , Doenças dos Peixes/microbiologia , Doenças dos Peixes/mortalidade , Doenças dos Peixes/patologia , Infecções por Bactérias Gram-Negativas/mortalidade , Infecções por Bactérias Gram-Negativas/patologia , Infecções por Bactérias Gram-Negativas/veterinária , Fatores Imunológicos/química , Fatores Imunológicos/farmacologia , Levofloxacino/análise , Levofloxacino/farmacologia , Testes de Sensibilidade Microbiana , Oligossacarídeos/farmacologia , Prebióticos , Taxa de Sobrevida
10.
Braz. J. Pharm. Sci. (Online) ; 58: e18630, 2022. tab, graf
Artigo em Inglês | LILACS | ID: biblio-1364418

RESUMO

Abstract The objective of the present investigation was to design, optimize and characterize the gastro retentive floating levofloxacin tablets and perform in-vivo evaluation using radiographic imaging. The floating tablets were prepared by using polymers i.e hydroxy propyl methyl cellulose (HPMC-K4M) and carbopol-940 individually and in combination by nonaquous granulation method. All the Formulations were evaluated for swelling index (S.I), floating behavior and in-vitro drug release kinetics. The compatibility study of levofloxacin with other polymers was investigated by FTIR, DSC, TGA and XRD. Results from FTIR and DSC revealed no chemical interaction amongst the formulation components. The optimized formulation (F11) showed floating lag time (FLT), total floating time (TFT) swelling index (S.I) of 60 sec, >16h and approximately 75 %, respectively. Moreover, F11 showed zero order levofloxacin release in simulated gastric fluid over the period of 6 h. X-ray studies showed that total buoyancy time was able to delay the gastric emptying of levofloxacin floating tablets in rabbits for more than 4 hours. In conclusion the optimized formulation (F11) can be used for the sustained delivery of levofloxacin for the treatment of peptic ulcer.


Assuntos
Liberação Controlada de Fármacos , Úlcera Péptica/classificação , Comprimidos/farmacologia , Raios X/efeitos adversos , Técnicas In Vitro/instrumentação , Espectroscopia de Infravermelho com Transformada de Fourier , Composição de Medicamentos/instrumentação , Otimização de Processos/análise , Levofloxacino/análise , Esvaziamento Gástrico/efeitos dos fármacos
11.
Bioanalysis ; 13(13): 1063-1070, 2021 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-34100294

RESUMO

Aim: A new HPLC method with fluorescence detection has been developed and validated for the determination of levofloxacin, one of the fluoroquinolone class antibiotics, in breast milk. Materials & methods: Chromatographic separation was carried out on a reversed phase C18 column with acetonitrile and 10 mM o-phosphoric acid (25:75, v/v) mobile phase composition. Moxifloxacin was used as internal standard and the peaks were detected by fluorescence detection. Results & conclusion: Calibration graph was found linearly within the range of 2.5-500 ng/ml. Limit of detection and limit of quantification were found to be 0.63 and 2.11 ng/ml, respectively. Mean absolute recovery was 96.18%. The developed method has been successfully applied to the determination of levofloxacin in human breast milk taken from two healthy volunteers.


Assuntos
Antibacterianos/análise , Cromatografia Líquida de Alta Pressão/métodos , Fluoroquinolonas/análise , Levofloxacino/análise , Leite Humano/química , Adulto , Calibragem , Feminino , Fluorescência , Humanos , Moxifloxacina/análise , Reprodutibilidade dos Testes
12.
Anal Bioanal Chem ; 413(16): 4329-4339, 2021 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-34041574

RESUMO

A reliable and efficient method for the simultaneous extraction and determination of antibiotics of ciprofloxacin and levofloxacin from milk was developed with solid phase extraction based on tailored adsorbent materials of deep eutectic solvents modified phenolic resin (DES-R-SPE). Six types of polyhydric alcohol-based hydrophilic DESs were prepared to modify the phenolic resin with the compositions of 3-aminophenol as a functional monomer, glyoxylic acid as a crosslinker, and polyethylene glycol 6000 as a porogen. And the prepared DES-Rs showed better extraction capacities for the target analytes than the unmodified phenolic resin because of more hydrogen bonding and electrostatic interactions supplied by DESs. The choline chloride-glycerol-based resin (DES1-R) with the highest adsorption amounts was selected and the adsorption behavior of it was studied with static adsorption and the dynamic adsorption performance; the adsorption process followed Freundlich isotherm (R2 ≥ 0.9337) and pseudo-second-order (R2 ≥ 0.9951). The present DES1-R-SPE method showed good linear range from 0.5 to100 µg mL-1 (R2 ≥ 0.9998), good recoveries of spiked milk samples (LEV, 96.7%; CIP, 101.5%), and satisfied repeatability for intra-day and inter-day (LEV, RSD≤5.4%; CIP, RSD≤4.6%).


Assuntos
Antibacterianos/isolamento & purificação , Ciprofloxacina/isolamento & purificação , Contaminação de Alimentos/análise , Formaldeído/química , Levofloxacino/isolamento & purificação , Leite/química , Fenóis/química , Polímeros/química , Adsorção , Animais , Antibacterianos/análise , Ciprofloxacina/análise , Interações Hidrofóbicas e Hidrofílicas , Levofloxacino/análise , Extração em Fase Sólida/métodos , Solventes
13.
Inorg Chem ; 60(9): 6585-6599, 2021 May 03.
Artigo em Inglês | MEDLINE | ID: mdl-33878862

RESUMO

Silver vanadate nanorods (ß-AgVO3) with silver nanoparticles (Ag-NPs) decorated on the surface of the rods were synthesized by using simple hydrothermal technique and later anchored onto nitrogen-doped reduced graphene oxide (N-rGO) to make a novel nanocomposite. Experimental analyses were carried out to identify the electronic configuration by X-ray diffraction analysis, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy analysis, which revealed monoclinic patterns of the C12/m1 space group with Wulff construction forming beta silver vanadate (ß-AgVO3) crystals with optical density and phase transformations. Ag nucleation showed consistent results with metallic formation and electronic changes occurring in [AgO5] and [AgO3] clusters. Transmission electron microscopy and field-emission scanning electron microscopy with elemental mapping and EDX analysis of the morphology reveals the nanorod structure for ß-AgVO3 with AgNPs on the surface and sheets for N-rGO. Additionally, a novel electrochemical sensor is constructed by using Ag/AgVO3/N-rGO on screen-printed carbon paste electrodes for the detection of antiviral drug levofloxacin (LEV) which is used as a primary antibiotic in controlling COVID-19. Using differential pulse voltammetry, LEV is determined with a low detection limit of 0.00792 nm for a linear range of 0.09-671 µM with an ultrahigh sensitivity of 152.19 µA µM-1 cm-2. Furthermore, modified electrode performance is tested by real-time monitoring using biological and river samples.


Assuntos
Espectroscopia Dielétrica/instrumentação , Espectroscopia Dielétrica/métodos , Levofloxacino/análise , Nanocompostos/química , Antivirais/análise , Antivirais/sangue , Antivirais/urina , Carbono/química , Eletrodos , Grafite/química , Humanos , Levofloxacino/sangue , Levofloxacino/urina , Limite de Detecção , Nanopartículas Metálicas/química , Microscopia Eletrônica de Transmissão , Nanotubos/química , Espectroscopia Fotoeletrônica , Prata/química , Compostos de Prata/química , Espectroscopia de Infravermelho com Transformada de Fourier , Análise Espectral Raman , Comprimidos , Vanadatos/química , Difração de Raios X
14.
Anal Chem ; 92(5): 3636-3642, 2020 03 03.
Artigo em Inglês | MEDLINE | ID: mdl-32011123

RESUMO

We developed a J-compensated QHSQC NMR method for the quantitative measurement of enantiopurity and concentration of levofloxacin in a complex drug matrix. The pulse sequence can achieve uniform signal responses by the suppression of the heteronuclear coupling modulation and alleviation of the homonuclear coupling evolution. Furthermore, we discuss the influence of relaxation on peak intensities and propose the selection conditions of reference signals to achieve accurate quantifications. The evaluation of the methodology shows that the results obtained by selected peaks are in accordance with theoretical analysis with good reliability and linearity. The enantiomeric separation and quantification of levofloxacin in creams are achieved by using a chiral solvating agent, a reference compound, and the J-compensated QHSQC pulse sequence. To our knowledge, this is the first example of QHSQC methodology to quantify enantiomers in the complex matrix.


Assuntos
Levofloxacino/análise , Levofloxacino/química , Espectroscopia de Ressonância Magnética/métodos , Modelos Lineares , Reprodutibilidade dos Testes , Estereoisomerismo
15.
J Sep Sci ; 43(3): 639-647, 2020 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-31705607

RESUMO

A novel green hydrophilic levofloxacin imprinted polymer was presented via one-step polymerization in water using ionic liquid 1,6-hexa-3,3'-bis-1-vinylimidazolium bromine with multiple hydrophilic groups and 2-hydroxyethyl methacrylate as a co-functional monomer. Adsorption experiment revealed that the ionic liquid significantly improved the water compatible of imprinted polymer, and the excellent recognition of molecularly imprinted polymer for levofloxacin in water corresponds to the synergetic effect of H-bonding and the electrostatic and π-π interactions between the levofloxacin and co-functional monomer. Furthermore, the adsorption process of the imprinted material towards levofloxacin fitted the Langmuir model, and the maximum binding amount of levofloxacin onto the imprinted and corresponding non-imprinted polymer were 16.45 and 6.82 mg/g at 25°C, respectively. After optimizing the parameters affecting solid phase extraction performance, an enrichment and determination system was achieved to separate and detect levofloxacin from water and sediment samples with recoveries that ranged from 83.67 to 101.33% and relative standard deviation of less than 5.59%.


Assuntos
Líquidos Iônicos/química , Levofloxacino/análise , Polímeros/química , Poluentes Químicos da Água/análise , Água/química , Interações Hidrofóbicas e Hidrofílicas , Estrutura Molecular
16.
Spectrochim Acta A Mol Biomol Spectrosc ; 220: 117153, 2019 Sep 05.
Artigo em Inglês | MEDLINE | ID: mdl-31141774

RESUMO

Levofloxacin is a third-generation fluoroquinolone antimicrobials drug that inhibits bacterial DNA replication. Driven by huge profit, one kind of particular counterfeit, e.g., repackaged expired tablets, becomes very common especially in developing countries. The feasibility of identifying expired levofloxacin tablets by combining NIR spectroscopy with chemometrics was investigated. Five kinds of levofloxacin samples from different manufacturers were collected for experiment. Two types of expired mode were considered and a simple model-independent algorithm was used for feature selection. Principal component analysis (PCA) was used for exploratory analysis and simple discriminant analysis. Taking seventy samples as the target class, a final one-class model based on Data Driven Soft Independent Modeling by Class Analogy with abbreviation DD-SIMCA was constructed, which achieved 97% sensitivity and 100% specificity on the independent set composed of 34 unexpired and 128 expired tablets. These results confirm that the combination of NIR spectroscopy, feature selection and class-modeling is feasible for identifying the expired levofloxacin tablets. Such a method can be extended to the analysis of similar drugs.


Assuntos
Medicamentos Falsificados/análise , Levofloxacino/análise , Espectroscopia de Luz Próxima ao Infravermelho/métodos , Algoritmos , Medicamentos Falsificados/química , Estudos de Viabilidade , Levofloxacino/química , Modelos Químicos , Medicamentos sob Prescrição/análise , Medicamentos sob Prescrição/química , Análise de Componente Principal , Sensibilidade e Especificidade , Processamento de Sinais Assistido por Computador , Espectroscopia de Luz Próxima ao Infravermelho/estatística & dados numéricos , Comprimidos/análise , Comprimidos/química , Fatores de Tempo
17.
Environ Int ; 128: 77-88, 2019 07.
Artigo em Inglês | MEDLINE | ID: mdl-31029982

RESUMO

Iron nanoparticles encapsulated within boron and nitrogen co-doped carbon nanoshell (B/N-C@Fe) were synthesized through a novel and green pyrolysis process using melamine, boric acid, and ferric nitrate as the precursors. The surface morphology, structure, and composition of the B/N-C@Fe materials were thoroughly investigated. The materials were employed as novel catalysts for the activation of potassium monopersulfate triple salt (PMS) for the degradation of levofloxacin (LFX). Linear sweep voltammograms and quenching experiments were used to identify the mechanisms of PMS activation and LFX oxidation by B/N-C@Fe, where SO4- as well as HO were proved to be the main radicals for the reaction processes. This study also discussed how the fluvic acid and inorganic anions in the aqueous solutions affected the degradation of LFX and use this method to simulate the degradation in the real wastewater. The synthesized materials showed a high efficiency (85.5% of LFX was degraded), outstanding stability, and excellent reusability (77.7% of LFX was degraded in the 5th run) in the Fenton-like reaction of LFX. In view of these advantages, B/N-C@Fe have great potentials as novel strategic materials for environmental catalysis.


Assuntos
Carbono/química , Poluentes Ambientais , Nanopartículas de Magnetita/química , Nanoconchas/química , Poluentes Ambientais/análise , Poluentes Ambientais/química , Concentração de Íons de Hidrogênio , Levofloxacino/análise , Levofloxacino/química , Oxirredução
18.
Biomed Chromatogr ; 33(3): e4415, 2019 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-30357876

RESUMO

(RS)-Etodolac was isolated from commercial tablets and was purified and characterized to be used as racemic standard. A pair of diastereomeric derivatives was synthesized using (S)-levofloxacin as a chiral derivatizing reagent. The derivatization reaction was carried out under conditions of stirring at room temperature (30°C for 1.5 h) as well as under microwave irradiation; the derivatives obtained by the two methods were compared. Reaction conditions for derivatization were optimized with respect to mole ratio of chiral derivatizing reagent and (RS)-etodolac. No racemization was observed throughout the study. Separation of diastereomeric derivatives was successful using C18 column and a binary mixture of methanol and triethyl ammonium phosphate buffer of pH 4.5 (80:20, v/v) as mobile phase at a flow rate of 1 mL min-1 and UV detection at 223 nm. An efficient approach for recognizing chirality and determining the absolute configuration of the diastereomeric derivatives of (RS)-etodolac is described, which in turn is a measure of the enantiomeric purity of (RS)-etodolac since the diastereomeric derivatives were separated and isolated using preparative thin-layer chromatography.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Cromatografia em Camada Fina/métodos , Etodolac/isolamento & purificação , Levofloxacino/isolamento & purificação , Etodolac/análise , Etodolac/química , Levofloxacino/análise , Levofloxacino/química , Limite de Detecção , Modelos Moleculares , Reprodutibilidade dos Testes , Estereoisomerismo
19.
Analyst ; 143(17): 4128-4135, 2018 Aug 20.
Artigo em Inglês | MEDLINE | ID: mdl-30062338

RESUMO

Early disease diagnosis is crucial for timely and effective healthcare monitoring and treatment. Demand for modern point-of-care (POC) technologies has increased during the past decade. Continuous monitoring of patient health status can be achieved through wearable sensors which can be incorporated into clothing and other wearables. While electronic textiles that monitor physical parameters (heart rate, blood pressure, etc.) are increasingly commonplace, smart textiles capable of monitoring chemical biomarkers are much less common. In this work, a conductive plasmonic electrochemical sensor was developed from a cotton blend fabric modified with silver nanoparticles and conductive inks. para-Aminothiophenol (pATP) was used as an initial probe molecule to evaluate the performance of the fabric-based electrode for electrochemical surface-enhanced Raman spectroscopic (EC-SERS) measurements. Further investigation was then carried out to detect levofloxacin, a commonly prescribed antibiotic, in both 0.1 M NaF and synthetic urine as supporting electrolyte. It was found that the fabric-based electrode provided excellent EC-SERS signals, comparable to commercial screen-printed electrodes, allowing for rapid detection of levofloxacin at clinically relevant concentrations. To the best of our knowledge, this is the first time a fabric-based electrode has been reported for EC-SERS investigations, highlighting a promising platform for wearable point-of-care sensors.


Assuntos
Sistemas Automatizados de Assistência Junto ao Leito , Análise Espectral Raman , Técnicas Eletroquímicas , Desenho de Equipamento , Humanos , Tinta , Levofloxacino/análise , Nanopartículas Metálicas , Prata , Têxteis , Dispositivos Eletrônicos Vestíveis
20.
Chemosphere ; 198: 174-181, 2018 May.
Artigo em Inglês | MEDLINE | ID: mdl-29421727

RESUMO

The degradation of solutions of the antibiotic levofloxacin (LVN) in sulfate medium at pH 3.0 has been investigated at pre-pilot scale by solar photoelectro-Fenton (SPEF) process. The flow plant included an FM01-LC filter-press cell equipped with a Ti|Pt anode and a three-dimensional-like air-diffusion cathode, connected to a compound parabolic collector as photoreactor and a continuous stirred tank under recirculation batch mode. The effect of volumetric flow rate on H2O2 electrogeneration from O2 reduction was assessed. Then, the influence of initial LVN concentration and Fe2+ concentration as catalyst on dissolved organic carbon (DOC) removal was thoroughly investigated. LVN was gradually mineralized by SPEF process, with faster DOC abatement at 0.50 mM Fe2+, yielding 100% after 360 min at applied cathodic potential of -0.30 V|SHE. The high mineralization current efficiency (MCE) and low specific energy consumption (ECDOC) revealed the extraordinary role of homogeneous hydroxyl radicals and natural UV light, which allowed the degradation of the antibiotic and its by-products with MCE values greater than 100%. Five cyclic by-products, N,N-diethylformamide and three short-chain linear carboxylic acids were detected by GC-MS and HPLC analyses. A parametric model to simulate the DOC decay versus electrolysis time was implemented for the SPEF pre-pilot flow plant, showing good agreement with experimental data.


Assuntos
Antibacterianos/análise , Peróxido de Hidrogênio/química , Ferro/química , Levofloxacino/análise , Modelos Teóricos , Raios Ultravioleta , Poluentes Químicos da Água/análise , Purificação da Água/métodos , Antibacterianos/efeitos da radiação , Catálise , Relação Dose-Resposta a Droga , Técnicas Eletroquímicas , Levofloxacino/efeitos da radiação , Projetos Piloto , Solubilidade , Fatores de Tempo , Poluentes Químicos da Água/efeitos da radiação
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