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1.
Ecotoxicol Environ Saf ; 186: 109778, 2019 Dec 30.
Artículo en Inglés | MEDLINE | ID: mdl-31627095

RESUMEN

Freshness protection packages and preservative films are widely used food-contact plastic made of polyethylene. Diode array detector (DAD), charged aerosol detector (CAD) and evaporative light-scattering detector (ELSD) were evaluated for determination of 6 bisphenols (bisphenol A, bisphenol S, bisphenol F, bisphenol B, bisphenol AF and tetrabromobisphenol A.) in polyethylene. DAD presented better parameters including limit of quantification (LOQs) ranging from 0.05 to 0.5 µg/g with relative standard deviations (RSDs, n = 5) lower than 1% at two concentration levels. CAD and ELSD are universal detectors with relative consistent response parameters for different analogues which have potential application by using single calibrant for quantification of multiple analytes. Matrix effects were barely observed on three detectors. Samples of freshness protection packages and preservative films were further analyzed and preliminary profiles of bisphenols in products from Beijing market was obtained. Bisphenol S have become most abundant analogue instead of bisphenol A in investigated products.


Asunto(s)
Compuestos de Bencidrilo/análisis , Cromatografía Líquida de Alta Presión/métodos , Embalaje de Alimentos , Fenoles/análisis , Polietileno/química , Sulfonas/análisis , Cromatografía Líquida de Alta Presión/instrumentación , Límite de Detección
2.
J Environ Sci Health B ; 53(2): 116-120, 2018 Feb 01.
Artículo en Inglés | MEDLINE | ID: mdl-29172986

RESUMEN

A simple and sensitive validated analytical method based on liquid chromatography coupled to tandem fluorescence (FD) and ultraviolet (UV) spectrophotometry was applied to monitor the presence of bisphenol A and bisphenol S in plastic baby bottles marketed in Italy. The limits of detection (LOD) were 3.75 ng mL-1 and 80.00 ng mL-1, and those of quantification (LOQ) were 12.51 ng mL-1 and 260.00 ng mL-1 for BPA (FD detection) and for BPS (UV detection), respectively. BPA was found in only four samples, two samples undergone to microwave heating and two samples undergone to bottle warmer heating either at 40°C or at 80°C. Although the quantities of leached BPA were well below the reference dose for daily intake established by the European Food Safety Authority (EFSA) (4.0 µg kg-1 bw/day), the release of BPA and BPS from these plastic materials should be carefully considered by the government authorities to increase people's awareness on this issue and to protect the most vulnerable population group.


Asunto(s)
Compuestos de Bencidrilo/análisis , Contaminación de Alimentos/análisis , Embalaje de Alimentos , Leche/química , Fenoles/análisis , Sulfonas/análisis , Animales , Cromatografía Liquida/métodos , Fluorescencia , Humanos , Lactante , Italia , Límite de Detección , Microondas , Plásticos/química , Espectrofotometría Ultravioleta/métodos
4.
Environ Sci Pollut Res Int ; 31(39): 51844-51857, 2024 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-39129044

RESUMEN

Passive sampling is a crucial method for evaluating concentrations of hydrophilic organic compounds in the aquatic environment, but it is insufficiently understood to what extent passive samplers capture the intermittent emissions that frequently occur for this group of compounds. In the present study, silicone sheets and styrene-divinyl benzene-reversed phase sulfonated extraction disks with and without a polyethersulfone membrane were exposed under semi-field conditions in a 31 m3 flume at three different flow velocities. Natural processes and spiking/dilution measures caused aqueous concentrations to vary strongly with time. The data were analyzed using two analytical models that account for these time-variable concentrations: a sampling rate model and a diffusion model. The diffusion model generally gave a better fit of the data than the sampling rate model, but the difference in residual errors was quite small (median errors of 19 vs. 25% for silicone and 22 vs. 25% for SDB-RPS samplers). The sampling rate model was therefore adequate enough to evaluate the time-integrative capabilities of the samplers. Sampler performance was best for SDB-RPS samplers with a polyethersulfone membrane, despite the occurrence of lag times for some compounds (0.1 to 0.4 days). Sampling rates for this design also spanned a narrower range (80 to 110 mL/day) than SDB-RPS samplers without a membrane (100 to 660 mL/day). The effect of biofouling was similar for all compounds and was consistent with a biofouling layer thickness of 150 µm.


Asunto(s)
Monitoreo del Ambiente , Interacciones Hidrofóbicas e Hidrofílicas , Contaminantes Químicos del Agua , Contaminantes Químicos del Agua/análisis , Monitoreo del Ambiente/métodos , Sulfonas/química , Sulfonas/análisis , Polímeros
5.
Environ Pollut ; 246: 452-462, 2019 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-30583153

RESUMEN

Marine polychaetes and fish are known to ingest polystyrene microparticles in the environment. Laboratory microplastic feeding experiments have demonstrated that plastic may release endocrine-disrupting compounds such as diethylhexyl phthalate (DEHP), which can cause adverse effects in both vertebrates and invertebrates. In order to determine the influence of size and digestive conditions on the desorption of DEHP and other plasticizers to polychaetes and fish, we exposed polystyrene particles of various sizes under invertebrate and vertebrate digestive conditions (vertebrate mimic; pepsin, pH = 2.0, 24 °C, invertebrate mimic; Na taurocholate pH = 7, 18 °C). Estrogen receptor activation and concentrations of 12 plasticizers were measured in the extracts. DEHP, bisphenol S and 4-tert-octylphenol were the only compounds detected. Simulated vertebrate gut digestion did not significantly enhance the release of chemicals nor estrogenic activity. However, a 6.3 ±â€¯2.0-fold increase in the concentration of DEHP was observed in extracts from invertebrate gut conditions (Mean ±â€¯SD; N = 24, p < 0.0001). Additionally, estimated particle surface area was positively correlated with estrogenic activity across all treatment types (r = 0.85, p < 0.0001). Overall, these data indicate an elevated bioaccessibility of DEHP may occur in invertebrates, and size-dependent desorption of uncharacterized estrogenic compounds from plastic suggest additional complexity when considering the risks of MP to aquatic organisms.


Asunto(s)
Dietilhexil Ftalato/toxicidad , Estrógenos/metabolismo , Peces/metabolismo , Plastificantes/toxicidad , Poliquetos/efectos de los fármacos , Poliquetos/metabolismo , Poliestirenos/toxicidad , Animales , Organismos Acuáticos/efectos de los fármacos , Línea Celular , Dietilhexil Ftalato/análisis , Digestión/fisiología , Disruptores Endocrinos/química , Fenoles/análisis , Plastificantes/química , Poliestirenos/metabolismo , Receptores de Estrógenos/metabolismo , Sulfonas/análisis
6.
Artículo en Inglés | MEDLINE | ID: mdl-29537947

RESUMEN

Polyphenylsulfone (PPSU) is a new material for the production of baby bottles. PPSU is a polyether plastic formally composed of bisphenol S (BPS) and 4,4'-dihydroxybiphenyl (DHBP), which both have slight endocrine activities in in vitro tests. So far, little is known about the presence and the release of potentially hazardous substances from PPSU baby bottles. In this study, we present a three-step approach for the analysis of PPSU starting with polymer characterisation in terms of chemical structure, total oligomer content and hydrolytic stability. Second is the determination of extractables focussing on monomers, monomer derivatives, linear and cyclic oligomers below 1000 Da and residual solvent. Third is a risk assessment on migration-related substances in accordance to European Union plastics regulation no. 10/2011 based on triplicate consecutive migration experiments using official milk simulant 50% ethanol. We analysed five types of PPSU baby bottles from different brands as well as corresponding raw materials from different manufacturers by various analytical techniques (high-performance liquid chromatography (HPLC)-diode array detector /fluorescence detector/Corona/electrospray ionisation-MS, HPLC-size exclusion chromatography, gas chromatography-mass spectrometry (GC-MS), 1H-NMR). We found significant variations of PPSU materials from different producers with regard to polymer and oligomer chain end groups (methoxylation, chlorination), while total oligomer content below 1000 Da was similar (mean about 0.48%). BPS was not detected above 0.3 mg/kg polymer in any PPSU sample. Residual DHBP content ranged between 1.7 and 15.5 mg/kg polymer. The most common oligomer in all PPSU samples was the cyclic tetramer (about 1200 mg/kg polymer), which is the only cyclic compound below 1000 Da. Residual solvent, sulfolane, was determined to a maximum of 1300 mg/kg polymer. In migration tests, we detected exceedances of neither specific migration limits for listed substances nor of thresholds of toxicological concern for non-listed substances (monomer derivatives, oligomers). Based on our analytical results, no concerns exist regarding migration of polymer-related substances from PPSU baby bottles.


Asunto(s)
Contaminación de Alimentos/análisis , Embalaje de Alimentos , Plásticos/análisis , Polímeros/análisis , Sulfonas/análisis , Cromatografía en Gel , Cromatografía de Gases y Espectrometría de Masas , Humanos , Lactante , Polímeros/síntesis química , Espectrometría de Fluorescencia
7.
Biosens Bioelectron ; 100: 341-347, 2018 Feb 15.
Artículo en Inglés | MEDLINE | ID: mdl-28942347

RESUMEN

In this paper, a novel molecularly imprinted electrochemical sensor (MIECS) based on a glassy carbon electrode (GCE) modified with graphene quantum dots (GQDs) coated on hollow nickel nanospheres (hNiNS) for the rapid determination of bisphenol S (BPS) was proposed for the first time. HNiNS and GQDs as electrode modifications were used to enlarge the active area and electron-transport ability for amplifying the sensor signal, while molecularly imprinted polymer (MIP) film was electropolymerized by using pyrrole as monomer and BPS as template to detect BPS via cyclic voltammetry (CV). Scanning electron microscope (SEM), energy-dispersive spectrometry (EDS), CV and differential pulse voltammetry (DPV) were employed to characterize the fabricated sensor. Experimental conditions, such as molar ratio of monomer to template, electropolymerization cycles, pH, incubation time and elution time were optimized. The DPV response of the MIECS to BPS was obtained in the linear range from 0.1 to 50µM with a low limit of detection (LOD) of 0.03µM (S/N = 3) under the optimized conditions. The MIECS exhibited excellent response towards BPS with high sensitivity, selectivity, good reproducibility, and stability. In addition, the proposed MIECS was also successfully applied for the determination of BPS in the plastic samples with simple sample pretreatment.


Asunto(s)
Técnicas Electroquímicas/métodos , Impresión Molecular/métodos , Nanosferas/química , Níquel/química , Fenoles/análisis , Puntos Cuánticos/química , Sulfonas/análisis , Técnicas Biosensibles/economía , Técnicas Biosensibles/métodos , Técnicas Electroquímicas/economía , Grafito/química , Límite de Detección , Impresión Molecular/economía , Nanosferas/ultraestructura , Plásticos/química , Puntos Cuánticos/ultraestructura , Factores de Tiempo , Contaminantes Químicos del Agua/análisis
8.
Sci Total Environ ; 578: 392-398, 2017 Feb 01.
Artículo en Inglés | MEDLINE | ID: mdl-27838055

RESUMEN

The uptake calibration of three passive samplers, stir-bars, MESCO/stir-bars and polyethersulfone tubes (PESt), was assessed in seawater at different salinities for 17 organic compounds including organochlorine compounds, pesticides, phthalates, musk fragrances and triclosan. The calibration procedure was accomplished by exposing the samplers to a continuous flow of fortified seawater for up to 14days under laboratory conditions. Prior to the exposure, stir-bars and MESCO/stir-bars were loaded with a known amount of deuterated PAH mixture as performance reference compounds (PRC). For most of the studied compounds, the sampling rates (Rs, mL·day-1) were determined for each sampler at two salinities (15 and 30‰) and two nominal concentrations (25 and 50ng·L-1). Among the tested devices, though PES can be an outstanding cheap alternative to other passive samplers, naked or free stir-bars provided the best results in terms of uptake rates (i.e., the Rs values ranged from 30 to 350mL·day-1). Regarding the variation of the salinity, the Rs values obtained with naked stir-bars were statistically comparable in the full range of salinities (0-30‰) but the values obtained with MESCO/stir-bars and PESt were salinity dependent. Consequently, only stir-bars assured the required robustness to be used as passive samplers in intertidal estuarine environments. Finally, the stir-bars were applied to estimate the time-weighted average concentration of some of those contaminants in the feeding seawater of the experimental aquaria at the Plentzia Marine Station (Basque Country) and low levels of musks fragrances (0.1-0.2ng·L-1) were estimated.


Asunto(s)
Dimetilpolisiloxanos/análisis , Monitoreo del Ambiente , Estuarios , Polímeros/análisis , Sulfonas/análisis , Contaminantes Químicos del Agua/análisis , Compuestos Orgánicos , España
9.
J Chromatogr A ; 1517: 35-43, 2017 Sep 29.
Artículo en Inglés | MEDLINE | ID: mdl-28859891

RESUMEN

The present work presents a novel and rapid analytical method for the simultaneous analysis of bisphenol A (BPA), bisphenol B (BPB), bisphenol F (BPF) and bisphenol S (BPS) in edible oil based on dispersive micro solid phase extraction (DMSPE) for the first time followed by isotope dilution-ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The edible oil sample was dispersed by n-hexane and extracted with ammoniated methanol-water solution. Then the target analytes were dispersedly absorbed using the polymer anion exchange (PAX) as the sorbent and eluted by acidic methanol. After that, four bisphenols were separated on a C18 column by gradient elution with methanol and 0.05% ammonium hydroxide in water as mobile phase, detected by MS/MS under multiple reactions monitoring (MRM) mode and quantified by internal standard method. The PAX amounts, adsorption time, concentrations of formic acid in the elution solvent and volume of elution solvent for the DMSPE technique were optimized. The limit of detection and quantitation (LOD and LOQ), matrix effect, recovery and precision of the developed method were investigated. Results indicated that BPS and the rest three bisphenols displayed excellent linearity in the concentration ranges of 0.1-50µg/L and 0.5-250µg/L, respectively, with correlation coefficients (R2) all larger than 0.998. Achieved MLODs (S/N=3) varied between 0.1-0.4µg/kg for all bisphenols. The mean recoveries at three spiked levels in edible oil were in the range of 87.3-108%. Intra-day precision (n=6) and inter-day precision (n=5) were <9% and <11%, respectively. This method is of rapid-and-simple pretreatment, accurate and sensitive, and suitable for the simultaneous determination of bisphenols in edible oil.


Asunto(s)
Compuestos de Bencidrilo/análisis , Grasas Insaturadas en la Dieta/análisis , Análisis de los Alimentos/métodos , Polímeros/química , Extracción en Fase Sólida , Adsorción , Resinas de Intercambio Aniónico/química , Hexanos/química , Límite de Detección , Fenoles/análisis , Aceites de Plantas/química , Sulfonas/análisis , Espectrometría de Masas en Tándem
10.
Environ Sci Pollut Res Int ; 24(28): 22241-22250, 2017 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-28799066

RESUMEN

The dissipation kinetics, pre-harvest residue limits, and hazard quotient (HQ) assessments of the pesticides flubendiamide and fluopicolide were conducted for Korean melon (Cucumis melo L. var. makuwa) cultivated at two different sites. A single extraction and cleanup procedure was carried out using acetone (partitioned with dichloromethane) and amino solid-phase extraction cartridges, respectively. Residue analysis was performed by HPLC with ultraviolet detection. Both pesticides showed excellent linearity with correlation coefficients of 0.9999 and 0.9996 for flubendiamide and fluopicolide, respectively. The accuracy (expressed as recovery %) at three spiking levels was 92.0-103.6 and 82.8-105.3%, and the precision (expressed as relative standard deviation) was 1.7-3.4 and 2.7-5.3% for flubendiamide and fluopicolide, respectively. The initial residues of flubendiamide/fluopicolide were 0.326/0.376 and 0.206/0.298 mg/kg at sites 1 and 2, respectively. These amounts were substantially lower than the maximum residue limits (MRLs = 1 and 0.5 mg/kg for flubendiamide and fluopicolide, respectively) established by the Korean Ministry of Food and Drug Safety. The half-lives of flubendiamide were 5.8 and 6.5 days, and those of fluopicolide were 6.7 and 9.1 days at sites 1 and 2, respectively. The shorter half-lives were attributed to seasonal variations (higher temperatures) and enzymatic and metabolic profiling. The risk assessment HQs of flubendiamide were 0.217/0.249 on day 0, which decreased to 0.102/0.168 on day 5, and to 0.065/0.88 on day 10; the HQ values for fluopicolide were 0.029/0.042, 0.022/0.025, and 0.010/0.019 on day 0, day 5, and day 10, for sites 1/2, respectively. From this data, we concluded that the fruits could be consumed safely.


Asunto(s)
Benzamidas/análisis , Cucumis melo/química , Residuos de Plaguicidas/análisis , Sulfonas/análisis , Cromatografía Líquida de Alta Presión , Cucumis melo/crecimiento & desarrollo , Ambiente Controlado , Frutas/química , Frutas/crecimiento & desarrollo , Cinética , Plásticos/análisis , República de Corea , Medición de Riesgo , Extracción en Fase Sólida
11.
J Nanosci Nanotechnol ; 6(8): 2344-53, 2006 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-17037840

RESUMEN

New strategies aimed to surface modification of polymeric membranes are crucial to optimise cell-biomaterial interactions in vivo and in vitro biohybrid systems. In this paper, we investigated the surface modification of Polyethersulfone (PES) membranes by plasma polymerisation of acrylic acid monomers (PES-pdAA) and by immobilization of galactonic acid through a hydrophilic "spacer arm" molecule (PES-pdAA-SA-GAL). The modification steps were characterised by high resolution X-ray photoelectron spectroscopy. The performance of modified and unmodified membranes was evaluated by assessing the expression of liver specific biotransformation functions of pig and human hepatocytes. Human liver cells cultured on PES-pdAA-SA-GAL membranes displayed an enhanced albumin production, urea synthesis and protein secretion for 24 days of culture. The immobilisation of galactose derivative units on the membrane allowed specific interactions with hepatocytes biomimicking the cellular microenvironment and produced an improvement of the long-term maintenance and differentiation of human hepatocytes.


Asunto(s)
Materiales Biocompatibles/química , Galactosa/química , Hepatocitos/citología , Hígado/metabolismo , Nanotecnología/métodos , Polímeros/química , Sulfonas/química , Acrilatos/química , Animales , Biotransformación , Galactosa/análogos & derivados , Humanos , Lactonas/análisis , Membranas Artificiales , Azúcares Ácidos/química , Sulfonas/análisis , Propiedades de Superficie , Porcinos
12.
J Pharm Sci ; 105(12): 3520-3531, 2016 12.
Artículo en Inglés | MEDLINE | ID: mdl-27773525

RESUMEN

A significant number of therapeutic proteins are marketed as pre-filled syringes or other drug/device combination products and have been safely used in these formats for years. Silicone oil, which is used as lubricant, can migrate into the drug product and may interact with therapeutic proteins. In this study, particles in the size range of 0.2-5 µm and ≥1 µm as determined by resonant mass measurement and micro-flow imaging/light obscuration, respectively, resulted from silicone sloughing off the container barrel after agitation. The degree of droplet formation correlated well with the applied baked-on silicone levels of 13 µg and 94 µg per cartridge. Silicone migration was comparable in placebo, 2 mg/mL and 33 mg/mL IgG1 formulations containing 0.04% (w/v) polysorbate 20. Headspace substantially increased the formation of silicone droplets during agitation. The highest particle concentrations reached, however, were still very low compared to numbers described for spray-on siliconized containers. When applying adequate baked-on silicone levels below 100 µg, bake-on siliconization efficiently limits silicone migration into the drug product without compromising device functionality.


Asunto(s)
Anticuerpos Monoclonales/química , Química Farmacéutica/métodos , Inmunoglobulina G/química , Siliconas/química , Anticuerpos Monoclonales/análisis , Inmunoglobulina G/análisis , Tamaño de la Partícula , Soluciones Farmacéuticas/análisis , Soluciones Farmacéuticas/química , Polímeros/análisis , Polímeros/química , Siliconas/análisis , Espectroscopía Infrarroja por Transformada de Fourier/métodos , Sulfonas/análisis , Sulfonas/química
13.
J Anal Toxicol ; 40(1): 64-71, 2016.
Artículo en Inglés | MEDLINE | ID: mdl-26364317

RESUMEN

A novel solid-phase extraction method using activated carbon fiber (ACF) was developed and validated. ACF has a vast network of pores of varying sizes and microporous structures that result in rapid adsorption and selective extraction of sulfur mustard metabolites according to the pH of eluting solvents. ACF could not only selectively extract thiodiglycol and 1-methylsulfinyl-2-[2-(methylthio)-ethylsulfonyl]ethane eluting a 9:1 ratio of dichloromethane to acetone, and 1,1'-sulfonylbis[2-(methylsulfinyl)ethane] and 1,1'-sulfonylbis- [2-S-(N-acetylcysteinyl)ethane] eluting 3% hydrogen chloride in methanol, but could also eliminate most interference without loss of analytes during the loading and washing steps. A sample preparation method has been optimized for the extraction of sulfur mustard metabolites from human urine using an ACF sorbent. The newly developed extraction method was applied to the trace analysis of metabolites of sulfur mustard in human urine matrices in a confidence-building exercise for the analysis of biomedical samples provided by the Organisation for the Prohibition of Chemical Weapons.


Asunto(s)
Métodos Analíticos de la Preparación de la Muestra , Carbono/química , Sustancias para la Guerra Química/aislamiento & purificación , Gas Mostaza/aislamiento & purificación , Extracción en Fase Sólida/métodos , Acetona/química , Fibra de Carbono , Sustancias para la Guerra Química/metabolismo , Sustancias para la Guerra Química/toxicidad , Cromatografía Liquida , Humanos , Ácido Clorhídrico/química , Concentración de Iones de Hidrógeno , Metanol/química , Cloruro de Metileno/química , Gas Mostaza/metabolismo , Gas Mostaza/toxicidad , Sensibilidad y Especificidad , Compuestos de Sulfhidrilo/análisis , Sulfuros/análisis , Sulfonas/análisis , Sulfóxidos/análisis , Espectrometría de Masas en Tándem
14.
Mater Sci Eng C Mater Biol Appl ; 62: 113-22, 2016 May.
Artículo en Inglés | MEDLINE | ID: mdl-26952404

RESUMEN

The main aim of this work is to design a heat triggered transdermal drug delivery system (TDDS) using a thermoresponsive polymer, poly (N-vinyl caprolactam) [PNVCL] based gel, where in patients can themselves administer a pulse of drug on mere application of heat pad over the TDDS, whenever pain is experienced. The phase transition temperature of PNVCL was tuned to 35 °C by grafting it onto a pH sensitive biopolymer, Chitosan, to synthesize Chitosan-g-PNVCL (CP) co-polymer which render the gel both thermo- and pH-responsive property. The application of triggered delivery was explored by loading acetamidophenol (a model hydrophilic drug) and etoricoxib (a model hydrophobic drug). In vitro drug release experiments were performed at three different temperatures (25, 32 and 39 °C) at two different pH (5.5 and 7) to study its drug release with response to temperature and pH. Drug release profiles obtained were found to have enhanced release for both the drugs respectively at 39 °C (above LCST) and pH5.5 when compared to other release conditions. In vitro skin permeation of both the drugs performed in rat abdominal skin using Franz diffusion cell showed enhanced drug release when the skin was subjected to higher temperature (39 °C). Moreover, it was also found that skin permeation for hydrophobic drug was better than that of hydrophilic drug. The in vivo biocompatibility studies of the CP gel in rat skin proved that the gel is biocompatible. The results obtained demonstrated the potential use of the thermoresponsive CP gel as an on-demand localized drug delivery system.


Asunto(s)
Acetaminofén/química , Analgésicos no Narcóticos/química , Portadores de Fármacos/química , Geles/química , Polímeros/química , Piridinas/química , Sulfonas/química , Acetaminofén/análisis , Acetaminofén/farmacología , Administración Cutánea , Analgésicos no Narcóticos/análisis , Analgésicos no Narcóticos/farmacología , Animales , Materiales Biocompatibles/química , Rastreo Diferencial de Calorimetría , Línea Celular , Supervivencia Celular/efectos de los fármacos , Quitosano/química , Difusión , Portadores de Fármacos/toxicidad , Liberación de Fármacos , Etoricoxib , Concentración de Iones de Hidrógeno , Interacciones Hidrofóbicas e Hidrofílicas , Masculino , Ratones , Manejo del Dolor , Transición de Fase , Piridinas/análisis , Piridinas/farmacología , Ratas , Ratas Sprague-Dawley , Piel/efectos de los fármacos , Piel/metabolismo , Espectroscopía Infrarroja por Transformada de Fourier , Sulfonas/análisis , Sulfonas/farmacología , Temperatura de Transición
15.
AAPS PharmSciTech ; 6(3): E405-12, 2005 Oct 19.
Artículo en Inglés | MEDLINE | ID: mdl-16353998

RESUMEN

The basic objectives of this study were to prepare and characterize solid dispersions of poorly water-soluble drug etoricoxib using lipid carriers by spray drying technique. The properties of solid dispersions were studied by diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), differential scanning calorimetry (DSC), hot-stage microscopy (HSM), radiograph powder diffraction (XRPD), and dissolution studies. The absence of etoricoxib peaks in XRPD profiles of solid dispersions suggests the transformation of crystalline etoricoxib into an amorphous form. In the HSM examination of solid dispersions, the dissolution of drug in the lipid carriers was observed, which was also confirmed by the absence of etoricoxib peak in DSC curves of solid dispersions. The DRIFTS spectra revealed the presence of hydrogen bonding in solid dispersions. The in vitro dissolution test showed a significant increase in the dissolution rate of solid dispersions as compared with pure etoricoxib, spray-dried etoricoxib, and physical mixtures of drug with lipid carriers. Therefore, the dissolution rate of poorly water-soluble drug etoricoxib can be significantly enhanced by the preparation of solid dispersions using lipid carriers by spray drying technique.


Asunto(s)
Portadores de Fármacos/química , Piridinas/síntesis química , Sulfonas/síntesis química , Tecnología Farmacéutica/métodos , Química Farmacéutica , Portadores de Fármacos/análisis , Portadores de Fármacos/farmacocinética , Etoricoxib , Liposomas , Piridinas/análisis , Piridinas/farmacocinética , Solubilidad , Sulfonas/análisis , Sulfonas/farmacocinética
16.
Biointerphases ; 10(1): 019011, 2015 Mar 24.
Artículo en Inglés | MEDLINE | ID: mdl-25711334

RESUMEN

The surfaces of polymeric dialyzer membranes consisting of polysulfone and polyvinylpyrrolidone were investigated regarding the lateral distribution and quantitative surface composition using time-of-flight secondary-ion-mass-spectrometry and x-ray photoelectron spectroscopy. Knowledge of the distribution and composition on the outer surface region is of utmost importance for understanding the biocompatibility of such dialyzer membranes. Both flat membranes and hollow fiber membranes were studied.


Asunto(s)
Membranas/química , Espectroscopía de Fotoelectrones , Polímeros/análisis , Povidona/análisis , Espectrometría de Masa de Ion Secundario , Sulfonas/análisis , Propiedades de Superficie
17.
J Agric Food Chem ; 50(5): 1045-52, 2002 Feb 27.
Artículo en Inglés | MEDLINE | ID: mdl-11853478

RESUMEN

Dimethenamid [2-chloro-N-(2,4-dimethyl-3-thienyl)-N-(2-methoxy-1-methylethyl)acetamide] and flufenacet [N-(4-fluorophenyl)-N-(1-methylethyl)-2-(5-(trifluoromethyl)-1,3,4-thiadiazol-2-yl)oxy] were isolated by C-18 solid-phase extraction and separated from their ethanesulfonic acid (ESA) and oxanilic acid (OXA) degradates during their elution using ethyl acetate for the parent compound, followed by methanol for the polar degradates. The parent compounds were detected using gas chromatography-mass spectrometry in selected-ion mode. The ESA and OXA degradates were detected using high-performance liquid chromatography--electrospray mass spectrometry (HPLC-ESPMS) in negative-ion mode. The method detection limits for a 123-mL sample ranged from 0.01 to 0.07 microg/L. These methods are compatible with existing methods and thus allow for analysis of 17 commonly used herbicides and 18 of their degradation compounds with one extraction. In a study of herbicide transport near the mouth of the Mississippi River during 1999 and 2000, dimethenamid and its ESA and OXA degradates were detected in surface water samples during the annual spring flushes. For flufenacet, the only detections at the study site were for the ESA degradates in samples collected at the peak of the herbicide spring flush in 2000. The low frequency of detections in surface water likely is due to dimethenamid and flufenacet being relatively new herbicides. In addition, detectable amounts of the stable degradates have not been detected in ground water.


Asunto(s)
Acetamidas/análisis , Acetanilidas/análisis , Agua Dulce/análisis , Herbicidas/análisis , Ácido Oxámico/análogos & derivados , Tiadiazoles/análisis , Agua/análisis , Cromatografía Líquida de Alta Presión/métodos , Cromatografía de Gases y Espectrometría de Masas/métodos , Indicadores y Reactivos , Modelos Moleculares , Estructura Molecular , Ácido Oxámico/análisis , Sulfonas/análisis
18.
J Nanosci Nanotechnol ; 4(8): 976-81, 2004 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-15656189

RESUMEN

The interaction of single wall carbon nanotubes (SWNT) with an aqueous solution of the fully sulfonated polyaniline poly(2-methoxyaniline-5-sulfonic acid) (PMAS) and (+)-1-phenylethylamine (PhEA) has been investigated using spectroscopic methods. UV-vis spectral measurements show that the PMAS backbone undergoes conformational changes upon interaction with both SWNT and PhEA. Partial intercalation of PMAS into SWNTbundles was confirmed by Raman spectroscopy and electron microscopy.


Asunto(s)
Cristalización/métodos , Nanotecnología/métodos , Nanotubos de Carbono/química , Nanotubos de Carbono/ultraestructura , Fenetilaminas/química , Polímeros/química , Análisis Espectral , Sulfonas/química , Adsorción , Ensayo de Materiales , Conformación Molecular , Nanotecnología/instrumentación , Fenetilaminas/análisis , Polímeros/análisis , Sulfonas/análisis
19.
ASAIO J ; 48(1): 45-56, 2002.
Artículo en Inglés | MEDLINE | ID: mdl-11820220

RESUMEN

The surface features, morphology, and tensile properties of fibers obtained from pristine, reprocessed, and reused Fresenius Polysulfone High-Flux (Hemoflow F80A) hemodialyzers have been studied. Scanning electron microscopy of the dialyzer fibers revealed a dense skin layer on the inner surface of the membrane and a relatively thick porous layer on the outer surface. Transmission electron microscopy and atomic force microscopy showed an alteration in membrane morphology due to reprocessing and reuse, or to a deposition of blood-borne material on the membrane that is not removed with reprocessing. Fluorescent microscopy images also showed that a fluorescent material not removed by heat/citric acid reprocessing builds up with continued use of the dialyzers. The tensile properties of the dialyzer fibers were not affected by the heat/citric acid reprocessing procedure. The protein layers formed on pristine and reused hemodialyzer membranes during clinical use were also studied using sodium dodecyl sulfate polyacrylamide gel electrophoresis and immunoblotting. A considerable amount of protein was found on the blood side of single and multiple use dialyzers. Proteins adsorbed on the dialysate side of the membrane were predominantly in the molecular weight region below 30 kDa. Little protein was detected on the membranes of reprocessed hemodialyzers.


Asunto(s)
Anticoagulantes , Materiales Biocompatibles/análisis , Ácido Cítrico , Polímeros/análisis , Diálisis Renal/instrumentación , Sulfonas/análisis , Proteínas Sanguíneas/análisis , Electroforesis en Gel de Poliacrilamida , Equipo Reutilizado , Calor , Humanos , Immunoblotting , Fallo Renal Crónico/terapia , Membranas Artificiales , Microscopía de Fuerza Atómica , Microscopía Electrónica , Dodecil Sulfato de Sodio , Tensoactivos , Resistencia a la Tracción
20.
Int J Artif Organs ; 24(11): 757-64, 2001 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-11797845

RESUMEN

Modern dialysis membranes need to fulfil two basic requirements. Firstly, the membrane structure, defined in terms of the size, structure and distribution of the pores at the inner separating layer of the membrane must be such that uraemic solutes of a defined molecular-weight range are selectively removed. Secondly, the physical and chemical properties of the blood-contacting surface must be such that minimal blood-material interactions take place that could either affect the functioning of the membrane, or, cause adverse reactions for the patient. A new polysulfone dialysis membrane, Helixone, has been developed specifically for the elimination of larger uraemic toxins using convective therapy modalities such as haemodiafiltration. The membrane is characterised by the nanoscale modulation of the innermost surface structures that lead to significantly increased sieving coefficients for molecules such as beta2-microglobulin, while maintaining the extremely low albumin removal property of the high-flux Fresenius Polysulfone membrane. A recent publication (Ronco C, Bowry SK. Nanoscale modulation of the pore dimensions, size distribution and structure of a new polysulfone-based high-flux dialysis membrane. Int J Artif Organs 2001; 24: 726-35) described the characterisation of the membrane of Helixone in terms of the membrane wall structure- and permeation-related parameters. In this paper, we describe the analysis of membrane surface parameters that influence the biocompatibility as well as the functioning of a membrane. The degree of roughness and the type of chemical groups of a blood-contacting surface are two of the main determinants of the biocompatibility characteristics of a membrane. The surface elemental composition of Helixone was determined using electron spectroscopy for elemental analysis (ESCA) while the surface topography of the membrane was evaluated using atomic force microscopy (AFM). The analysis showed that Helixone has an improved, smoother blood-contacting surface and retains the essential surface chemistry, and therefore the acknowledged biocompatibility profile, of the Fresenius Polysulfone membrane.


Asunto(s)
Materiales Biocompatibles/análisis , Materiales Biocompatibles Revestidos/análisis , Membranas Artificiales , Polímeros/análisis , Diálisis Renal/instrumentación , Sulfonas/análisis , Humanos , Microscopía de Fuerza Atómica/métodos , Nanotecnología , Espectrometría por Rayos X/métodos , Propiedades de Superficie
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