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1.
Carbohydr Polym ; 340: 122306, 2024 Sep 15.
Artículo en Inglés | MEDLINE | ID: mdl-38858025

RESUMEN

In this study, a novel hydrogel, ß-cyclodextrin/carbon dots-grafted cellulose nanofibrils hydrogel (ßCCH), was fabricated for removal and fluorescence determination of levofloxacin (LEV). A comprehensive analysis was performed to characterize its physicochemical properties. Batch adsorption experiments were conducted, revealing that ßCCH reached a maximum adsorption capacity of 1376.9 mg/g, consistent with both Langmuir and pseudo-second-order models, suggesting that the adsorption process of LEV on ßCCH was primarily driven by chemical adsorption. The removal efficiency of ßCCH was 99.2 % under the fixed conditions (pH: 6, initial concentration: 20 mg/L, contact time: 300 min, temperature: 25 °C). The removal efficiency of ßCCH for LEV still achieved 97.3 % after five adsorption-desorption cycles. By using ßCCH as a fluorescent probe for LEV, a fast and sensitive method was established with linear ranges of 1-120 mg/L and 0.2-1.0 µg/L and a limit of detection (LOD) as low as 0.09 µg/L. The viability of ßCCH was estimated based on the economic analysis of the synthesis process and the removal of LEV, demonstrating that ßCCH was more cost-effective than commercial activated carbon. This study provides a novel approach for preparing a promising antibiotic detection and adsorption material with the advantages of stability, and cost-effectiveness.


Asunto(s)
Carbono , Celulosa , Hidrogeles , Levofloxacino , Nanofibras , beta-Ciclodextrinas , Levofloxacino/análisis , Levofloxacino/química , beta-Ciclodextrinas/química , Celulosa/química , Adsorción , Nanofibras/química , Carbono/química , Hidrogeles/química , Antibacterianos/análisis , Antibacterianos/química , Límite de Detección , Contaminantes Químicos del Agua/análisis , Colorantes Fluorescentes/química , Puntos Cuánticos/química , Fluorescencia
2.
Langmuir ; 40(24): 12671-12680, 2024 Jun 18.
Artículo en Inglés | MEDLINE | ID: mdl-38853520

RESUMEN

The design of single-atom nanozymes with dual active sites to increase their activity and for the detection and degradation of contaminants is rare and challenging. In this work, a single-atom nanozyme (FeCu-NC) based on a three-dimensional porous Fe/Cu dual active site was developed as a colorimetric sensor for both the quantitative analysis of isoniazid (INH) and the efficient degradation of levofloxacin (LEV). FeCu-NC was synthesized using a salt template and freeze-drying method with a three-dimensional hollow porous structure and dual active sites (Fe-Nx and Cu-Nx). In terms of morphology and structure, FeCu-NC exhibits excellent peroxidase-like activity and catalytic properties. Therefore, a colorimetric sensor was constructed around FeCu-NC for sensitive and rapid quantitative analysis of INH with a linear range of 0.9-10 µM and a detection limit as low as 0.3 µM, and the sensor was successfully applied to the analysis of INH in human urine. In addition, FeCu-NC promoted the efficient degradation of LEV by peroxymonosulfate activation, with a degradation rate of 90.4% for LEV at 30 min. This work sheds new light on the application of single-atom nanozymes to antibiotics for colorimetric sensing and degradation.


Asunto(s)
Cobre , Hierro , Isoniazida , Levofloxacino , Isoniazida/química , Isoniazida/análisis , Levofloxacino/orina , Levofloxacino/análisis , Levofloxacino/química , Hierro/química , Cobre/química , Humanos , Peroxidasa/química , Peroxidasa/metabolismo , Colorimetría/métodos , Nanoestructuras/química , Catálisis
3.
Inorg Chem ; 63(18): 8336-8341, 2024 May 06.
Artículo en Inglés | MEDLINE | ID: mdl-38651971

RESUMEN

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.


Asunto(s)
Alginatos , Europio , Levofloxacino , Zinc , Alginatos/química , Zinc/química , Zinc/sangre , Levofloxacino/sangre , Levofloxacino/análisis , Europio/química , Espectrometría de Fluorescencia , Animales , Humanos , Bovinos , Comprimidos , Colorantes Fluorescentes/química
4.
Int J Biol Macromol ; 267(Pt 1): 131321, 2024 May.
Artículo en Inglés | MEDLINE | ID: mdl-38570001

RESUMEN

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.


Asunto(s)
Compuestos Bicíclicos Heterocíclicos con Puentes , Quitosano , Técnicas Electroquímicas , Levofloxacino , Impresión Molecular , Polímeros Impresos Molecularmente , Polímeros , Quitosano/química , Levofloxacino/análisis , Levofloxacino/química , Polímeros/química , Compuestos Bicíclicos Heterocíclicos con Puentes/química , Impresión Molecular/métodos , Técnicas Electroquímicas/métodos , Polímeros Impresos Molecularmente/química , Electrodos , Límite de Detección , Humanos
5.
Chemosphere ; 355: 141763, 2024 May.
Artículo en Inglés | MEDLINE | ID: mdl-38522672

RESUMEN

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.


Asunto(s)
Ciprofloxacina , Contaminantes Químicos del Agua , Ciprofloxacina/química , Levofloxacino/análisis , Enoxacino/análisis , Diamante/química , Fluoroquinolonas/análisis , Piperazina , Oxidación-Reducción , Electrodos , Agua , Contaminantes Químicos del Agua/análisis
6.
Huan Jing Ke Xue ; 45(3): 1468-1479, 2024 Mar 08.
Artículo en Chino | MEDLINE | ID: mdl-38471862

RESUMEN

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.


Asunto(s)
Benzofenonas , Carbanilidas , Cosméticos , Triclosán , Contaminantes Químicos del Agua , Acetaminofén , Organismos Acuáticos , Cafeína/análisis , Ciprofloxacina , Cosméticos/análisis , Monitoreo del Ambiente/métodos , Levofloxacino/análisis , Preparaciones Farmacéuticas , Medición de Riesgo , Ríos/química , Aguas del Alcantarillado/análisis , Aguas Residuales , Contaminantes Químicos del Agua/análisis
7.
J Environ Manage ; 354: 120329, 2024 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-38373375

RESUMEN

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.


Asunto(s)
Contaminantes Ambientales , Contaminantes Químicos del Agua , Animales , Levofloxacino/análisis , Microplásticos/toxicidad , Plásticos , Tamaño de la Partícula , Intestinos/química , Encéfalo , Ranidae , Contaminantes Ambientales/análisis , Contaminantes Químicos del Agua/toxicidad , Contaminantes Químicos del Agua/análisis
8.
J Environ Manage ; 344: 118718, 2023 Oct 15.
Artículo en Inglés | MEDLINE | ID: mdl-37541001

RESUMEN

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.


Asunto(s)
Aguas Residuales , Contaminantes Químicos del Agua , Antibacterianos , Levofloxacino/análisis , Peróxido de Hidrógeno , Contaminantes Químicos del Agua/química , Boro/química , Diamante/química , Oxidación-Reducción , Electrodos
9.
Sci Total Environ ; 862: 160773, 2023 Mar 01.
Artículo en Inglés | MEDLINE | ID: mdl-36509275

RESUMEN

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.


Asunto(s)
Levofloxacino , Contaminantes Químicos del Agua , Levofloxacino/análisis , Arena , Porosidad , Polímeros , Adsorción , Contaminantes Químicos del Agua/química
10.
Bioresour Technol ; 351: 127025, 2022 May.
Artículo en Inglés | MEDLINE | ID: mdl-35307521

RESUMEN

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.


Asunto(s)
Levofloxacino , Contaminantes Químicos del Agua , Adsorción , Animales , Carbón Orgánico/química , Cinética , Levofloxacino/análisis , Estiércol , Espectroscopía Infrarroja por Transformada de Fourier , Porcinos , Contaminantes Químicos del Agua/química
11.
Artículo en Inglés | MEDLINE | ID: mdl-34801729

RESUMEN

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.


Asunto(s)
Aeromonas hydrophila/efectos de los fármacos , Antibacterianos/farmacología , Enfermedades de los Peces/tratamiento farmacológico , Infecciones por Bacterias Gramnegativas/tratamiento farmacológico , Nanopartículas/química , Alimentación Animal , Animales , Antibacterianos/análisis , Antioxidantes/metabolismo , Acuicultura , Quitosano/química , Quitosano/farmacología , Cíclidos/crecimiento & desarrollo , Cíclidos/microbiología , Enfermedades de los Peces/microbiología , Enfermedades de los Peces/mortalidad , Enfermedades de los Peces/patología , Infecciones por Bacterias Gramnegativas/mortalidad , Infecciones por Bacterias Gramnegativas/patología , Infecciones por Bacterias Gramnegativas/veterinaria , Factores Inmunológicos/química , Factores Inmunológicos/farmacología , Levofloxacino/análisis , Levofloxacino/farmacología , Pruebas de Sensibilidad Microbiana , Oligosacáridos/farmacología , Prebióticos , Tasa de Supervivencia
12.
Braz. J. Pharm. Sci. (Online) ; 58: e18630, 2022. tab, graf
Artículo en Inglés | LILACS | ID: biblio-1364418

RESUMEN

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.


Asunto(s)
Liberación de Fármacos , Úlcera Péptica/clasificación , Comprimidos/farmacología , Rayos X/efectos adversos , Técnicas In Vitro/instrumentación , Espectroscopía Infrarroja por Transformada de Fourier , Composición de Medicamentos/instrumentación , Optimización de Procesos/análisis , Levofloxacino/análisis , Vaciamiento Gástrico/efectos de los fármacos
13.
Bioanalysis ; 13(13): 1063-1070, 2021 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-34100294

RESUMEN

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.


Asunto(s)
Antibacterianos/análisis , Cromatografía Líquida de Alta Presión/métodos , Fluoroquinolonas/análisis , Levofloxacino/análisis , Leche Humana/química , Adulto , Calibración , Femenino , Fluorescencia , Humanos , Moxifloxacino/análisis , Reproducibilidad de los Resultados
14.
Anal Bioanal Chem ; 413(16): 4329-4339, 2021 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-34041574

RESUMEN

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%).


Asunto(s)
Antibacterianos/aislamiento & purificación , Ciprofloxacina/aislamiento & purificación , Contaminación de Alimentos/análisis , Formaldehído/química , Levofloxacino/aislamiento & purificación , Leche/química , Fenoles/química , Polímeros/química , Adsorción , Animales , Antibacterianos/análisis , Ciprofloxacina/análisis , Interacciones Hidrofóbicas e Hidrofílicas , Levofloxacino/análisis , Extracción en Fase Sólida/métodos , Solventes
15.
Inorg Chem ; 60(9): 6585-6599, 2021 May 03.
Artículo en Inglés | MEDLINE | ID: mdl-33878862

RESUMEN

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.


Asunto(s)
Espectroscopía Dieléctrica/instrumentación , Espectroscopía Dieléctrica/métodos , Levofloxacino/análisis , Nanocompuestos/química , Antivirales/análisis , Antivirales/sangre , Antivirales/orina , Carbono/química , Electrodos , Grafito/química , Humanos , Levofloxacino/sangre , Levofloxacino/orina , Límite de Detección , Nanopartículas del Metal/química , Microscopía Electrónica de Transmisión , Nanotubos/química , Espectroscopía de Fotoelectrones , Plata/química , Compuestos de Plata/química , Espectroscopía Infrarroja por Transformada de Fourier , Espectrometría Raman , Comprimidos , Vanadatos/química , Difracción de Rayos X
16.
Anal Chem ; 92(5): 3636-3642, 2020 03 03.
Artículo en Inglés | MEDLINE | ID: mdl-32011123

RESUMEN

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.


Asunto(s)
Levofloxacino/análisis , Levofloxacino/química , Espectroscopía de Resonancia Magnética/métodos , Modelos Lineales , Reproducibilidad de los Resultados , Estereoisomerismo
17.
J Sep Sci ; 43(3): 639-647, 2020 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-31705607

RESUMEN

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%.


Asunto(s)
Líquidos Iónicos/química , Levofloxacino/análisis , Polímeros/química , Contaminantes Químicos del Agua/análisis , Agua/química , Interacciones Hidrofóbicas e Hidrofílicas , Estructura Molecular
18.
Spectrochim Acta A Mol Biomol Spectrosc ; 220: 117153, 2019 Sep 05.
Artículo en Inglés | MEDLINE | ID: mdl-31141774

RESUMEN

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.


Asunto(s)
Medicamentos Falsificados/análisis , Levofloxacino/análisis , Espectroscopía Infrarroja Corta/métodos , Algoritmos , Medicamentos Falsificados/química , Estudios de Factibilidad , Levofloxacino/química , Modelos Químicos , Medicamentos bajo Prescripción/análisis , Medicamentos bajo Prescripción/química , Análisis de Componente Principal , Sensibilidad y Especificidad , Procesamiento de Señales Asistido por Computador , Espectroscopía Infrarroja Corta/estadística & datos numéricos , Comprimidos/análisis , Comprimidos/química , Factores de Tiempo
19.
Environ Int ; 128: 77-88, 2019 07.
Artículo en Inglés | MEDLINE | ID: mdl-31029982

RESUMEN

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.


Asunto(s)
Carbono/química , Contaminantes Ambientales , Nanopartículas de Magnetita/química , Nanocáscaras/química , Contaminantes Ambientales/análisis , Contaminantes Ambientales/química , Concentración de Iones de Hidrógeno , Levofloxacino/análisis , Levofloxacino/química , Oxidación-Reducción
20.
Biomed Chromatogr ; 33(3): e4415, 2019 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-30357876

RESUMEN

(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.


Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Cromatografía en Capa Delgada/métodos , Etodolaco/aislamiento & purificación , Levofloxacino/aislamiento & purificación , Etodolaco/análisis , Etodolaco/química , Levofloxacino/análisis , Levofloxacino/química , Límite de Detección , Modelos Moleculares , Reproducibilidad de los Resultados , Estereoisomerismo
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