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1.
Eur Neurol ; 71(1-2): 65-74, 2014.
Artigo em Inglês | MEDLINE | ID: mdl-24334999

RESUMO

BACKGROUND: Palliative techniques such as partial corpus callosotomy (CC) and vagus nerve stimulation (VNS) may be effective for adequate control of seizures in pharmacoresistant patients who are not candidates for resective surgery. OBJECTIVE: The objective of this study was to analyze the efficacy of the combination of these two techniques in patients where the first surgery had not achieved adequate control. MATERIALS AND METHODS: This is a retrospective review of 6 patients with refractory epilepsy in which both types of surgery were performed, CC and VNS. We analyzed variables such as age, sex, age at onset of epilepsy, seizure types, electroencephalogram and magnetic resonance imaging results, and number of pre- and postoperative seizures. RESULTS: Three patients first underwent VNS and then CC, and 3 patients were treated in reverse order. All patients had some improvement after the first surgery, but they continued to experience persistent falls, so a second palliative technique was used. The mean improvement after both surgeries was 89% (90% in patients first receiving CC and 87% in patients who first underwent VNS). CONCLUSIONS: In adequately studied patients who are not optimal candidates for resective surgery, palliative surgery is a choice. The combination of VNS and CC shows good results in our series, although the right order to perform both procedures has not been defined. These results should be confirmed in a larger group of patients.


Assuntos
Corpo Caloso/cirurgia , Epilepsia/cirurgia , Epilepsia/terapia , Convulsões/cirurgia , Convulsões/terapia , Estimulação do Nervo Vago , Adulto , Fatores Etários , Idade de Início , Encéfalo/patologia , Encéfalo/fisiopatologia , Eletroencefalografia , Epilepsia/patologia , Epilepsia/fisiopatologia , Feminino , Seguimentos , Humanos , Imageamento por Ressonância Magnética , Masculino , Pessoa de Meia-Idade , Procedimentos Neurocirúrgicos/métodos , Estudos Retrospectivos , Convulsões/patologia , Convulsões/fisiopatologia , Fatores Sexuais , Resultado do Tratamento , Adulto Jovem
2.
Anal Bioanal Chem ; 400(5): 1251-61, 2011 May.
Artigo em Inglês | MEDLINE | ID: mdl-21274519

RESUMO

Nowadays, there are new technologies in high-performance liquid chromatography columns available enabling faster and more efficient separations. In this work, we compared three different types of columns for the analysis of main soy isoflavones. The evaluated columns were a conventional reverse phase particle column, a fused-core particle column, and a monolithic column. The comparison was in terms of chromatographic parameters such as resolution, asymmetry, number of theoretical plates, variability of retention time, and peak width. The lower column pressure was provided by the monolithic column, although lower chromatographic performance was achieved. Conventional and fused-core particle columns presented similar pressure. Results also indicate that direct transfer between particle and monolithic columns is not possible requiring adjustment of conditions and a different method optimization strategy. The best chromatographic performance and separation speed were observed for the fused-core particle column. Also, the effect of sample solvent on the separation and peak shape was evaluated and indicated that monolithic column is the most affected especially when using higher concentrations of acetonitrile or ethanol. Sample solvent that showed the lowest effect on the chromatographic performance of the columns was methanol. Overall evaluation of methanol and acetonitrile as mobile phase for the separation of isoflavones indicated higher chromatographic performance of acetonitrile, although methanol may be an attractive alternative. Using acetonitrile as mobile phase resulted in faster, higher resolution, narrower, and more symmetric peaks than methanol with all columns. It also generated the lower column pressure and flatter pressure profile due to mobile phase changes, and therefore, it presents a higher potential to be explored for the development of faster separation methods.


Assuntos
Cromatografia Líquida de Alta Pressão/instrumentação , Glycine max/química , Isoflavonas/isolamento & purificação , Acetonitrilas , Cromatografia Líquida de Alta Pressão/métodos , Metanol , Pressão , Reprodutibilidade dos Testes , Solventes
3.
J Chromatogr A ; 1216(1): 2-29, 2009 Jan 02.
Artigo em Inglês | MEDLINE | ID: mdl-19041977

RESUMO

This manuscript provides a review of the actual state and the most recent advances as well as current trends and future prospects in sample preparation and analysis for the quantification of isoflavones from soybeans and soy foods. Individual steps of the procedures used in sample preparation, including sample conservation, extraction techniques and methods, and post-extraction treatment procedures are discussed. The most commonly used methods for extraction of isoflavones with both conventional and "modern" techniques are examined in detail. These modern techniques include ultrasound-assisted extraction, pressurized liquid extraction, supercritical fluid extraction and microwave-assisted extraction. Other aspects such as stability during extraction and analysis by high performance liquid chromatography are also covered.


Assuntos
Métodos Analíticos de Preparação de Amostras/métodos , Glycine max/química , Isoflavonas/análise , Extratos Vegetais/isolamento & purificação , Alimentos de Soja/análise , Extratos Vegetais/química , Reprodutibilidade dos Testes
4.
Food Funct ; 8(10): 3654-3663, 2017 Oct 18.
Artigo em Inglês | MEDLINE | ID: mdl-28914314

RESUMO

Consumers and the food industry are demanding healthier products. Expanded snacks with a high nutritional value were developed from different rice, pea and carob flour blends. The proximate composition, starch (total and resistant), amylose and amylopectin, dietary fiber (soluble and insoluble) contents, and the in vitro protein digestibility of different rice-legume formulations, were evaluated before and after the extrusion process. Compared with the corresponding non-extruded blends (control), the extrusion treatment did not change the total protein content, however, it reduced the soluble protein (61-86%), the fat (69-92%) and the resistant starch contents (100%). The total starch content of all studied blends increased (2-19%) after extrusion. The processing increased the in vitro protein digestibility, reaching values around 88-95% after extrusion. Total dietary fiber was reduced around 30%, and the insoluble fraction was affected to a larger extent than the soluble fraction by the extrusion process. Because of its balanced nutritional composition, high dietary fiber content, as well as low energy density, these novel gluten-free snack-like foods could be considered as functional foods and a healthier alternative to commercially available gluten-containing or gluten-free and low nutritional value snacks.


Assuntos
Fibras na Dieta/análise , Farinha/análise , Oryza/química , Pisum sativum/química , Amilopectina/análise , Amilopectina/metabolismo , Culinária , Fibras na Dieta/metabolismo , Digestão , Glutens/análise , Glutens/metabolismo , Humanos , Valor Nutritivo , Oryza/metabolismo , Pisum sativum/metabolismo , Lanches , Amido/análise , Amido/metabolismo
5.
Sci Rep ; 7(1): 6338, 2017 07 24.
Artigo em Inglês | MEDLINE | ID: mdl-28740128

RESUMO

New psychoactive substances have been rapidly growing in popularity in the drug market as non-illegal drugs. In the last few years, an increment has been reported on the use of synthetic alternatives to heroin, the synthetic opioids. Based on the information provided by the European Monitoring Centre for Drug and Drug Addiction, these synthetic opioids have been related to overdoses and deaths in Europe and North America. One of these opioids is the U-47700. A few months ago, U-47700 was scheduled in the U.S. and other countries, and other opioid derivatives have been appearing in order to replace it. One of these compounds is U-49900, an analog of U-47700. A white powder sample was obtained from an anonymous user in Spain. After an accurate characterization by gas chromatography-mass spectrometry, ultra-high performance liquid chromatography-high resolution mass spectrometry, nuclear magnetic resonance and single-crystal X-ray diffraction; and complemented by Fourier-transformed infrared spectroscopy, ultraviolet and circular dichroism spectrophotometry, the drug sample was unequivocally identified as U-49900. The information provided will be useful for the Early Warning System and forensic laboratories for future identifications of the U-49900, as well as in tentative identifications of other related opioids.


Assuntos
Analgésicos Opioides/análise , Benzamidas/análise , Drogas Ilícitas/análise , Analgésicos Opioides/química , Benzamidas/química , Cromatografia Líquida de Alta Pressão/métodos , Cristalografia por Raios X , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Drogas Ilícitas/química , Estrutura Molecular , Espanha , Espectroscopia de Infravermelho com Transformada de Fourier , Espectrometria de Massas em Tandem
6.
J Chromatogr A ; 1525: 145-151, 2017 Nov 24.
Artigo em Inglês | MEDLINE | ID: mdl-29031968

RESUMO

Compound-specific isotope analysis (CSIA) usually requires preparative steps (pretreatments, extraction, derivatization) to get amenable chromatographic analytes from bulk geological, biological or synthetic materials. Analytical pyrolysis (Py-GC/MS) can help to overcome such sample manipulation. This communication describe the results obtained by hyphenating analytical pyrolysis (Py-GC) with carbon isotope-ratio mass spectrometry (IRMS) for the analysis of a polylactic acid (PLA) a based bio-plastic extruded with variable quantities of a natural plant extract or oregano essential oil. The chemical structural information of pyrolysates was first determined by conventional analytical pyrolysis and the measure of δ13C in specific compounds was done by coupling a pyrolysis unit to a gas chromatograph connected to a continuous flow IRMS unit (Py-GC-C-IRMS). Using this Py-CSIA device it was possible to trace natural additives with depleted δ13C values produced by C3 photosystem vegetation (cymene: -26.7‰±2.52; terpinene: -27.1‰±0.13 and carvacrol: -27.5‰±1.80 from oregano and two unknown structures: -23.3‰±3.32 and -24.4‰±1.70 and butyl valerate: -24.1‰±3.55 from Allium spp.), within the naturally isotopically enriched bio-plastic backbone derived from corn (C4 vegetation) starch (cyclopentanones: -14.2‰±2.11; lactide enantiomers: -9.2‰±1.56 and larger polymeric units: -17.2‰±1.71). This is the first application of Py-CSIA to characterize a bio-plastic and is shown as a promising tool to study such materials, providing not only a fingerprinting, but also valuable information about the origin of the materials, allowing the traceability of additives and minimizing sample preparation.


Assuntos
Técnicas de Química Analítica/métodos , Embalagem de Alimentos , Cromatografia Gasosa-Espectrometria de Massas , Poliésteres/química , Isótopos de Carbono/análise , Cimenos , Monoterpenos/análise , Óleos Voláteis/análise , Extratos Vegetais/análise , Polímeros/química
7.
Seizure ; 48: 53-56, 2017 May.
Artigo em Inglês | MEDLINE | ID: mdl-28419947

RESUMO

PURPOSE: Eslicarbazepine-acetate (ESL) is a third generation antiepileptic drug licensed as adjunctive therapy in adults with focal seizures. Efficacy and safety of ESL have been established in real-life setting. However, data about outcomes in elderly patients are scarce. Primary endpoint was to evaluate outcomes of ESL in elderly patients. METHOD: This was a retrospective survey that included patients >65years with focal seizures who started ESL between January 2010 and July 2012 at 12 Spanish Hospitals. ESL was prescribed individually according to real-life practice. Efficacy and safety were evaluated over 1year. These patients were included within the bigger study ESLIBASE. RESULTS: We included 29 patients, most of them males (18). Mean age was 71.2 year-old and epilepsy evolution was 20 years. Eighteen were pharmacorresistant at baseline. At 12 months, the mean dose was 850mg/day, the retention rate 69%, the responder rate 62% and 24.1% were seizure-free. At 12 months, 16 patients (55.2%) had ≥1 adverse effect (AE), that led to discontinuation in 7 patients. Dizziness, nausea and ataxia were the most common AEs. The tolerability profile improved in 4/5 patients who switched from carbamazepine (CBZ) or oxcarbazepine (OXC) to ESL due to AEs. CONCLUSIONS: ESL was well-tolerated and effective in elderly patients in a real-life setting over 1year, with a dose around 800mg/day. AE effects improved in most of who switched from CBZ or OXC to ESL.


Assuntos
Anticonvulsivantes/uso terapêutico , Dibenzazepinas/uso terapêutico , Epilepsias Parciais/tratamento farmacológico , Idoso , Idoso de 80 Anos ou mais , Anticonvulsivantes/efeitos adversos , Dibenzazepinas/efeitos adversos , Feminino , Humanos , Masculino , Estudos Retrospectivos , Resultado do Tratamento
8.
Artigo em Inglês | MEDLINE | ID: mdl-27455176

RESUMO

Consumers' concerns about the environment and health have led to the development of new food packaging materials avoiding petroleum-based matrices and synthetic additives. The present study has developed polylactic acid (PLA) films containing different concentrations of essential oil from Origanum vulgare L. virens (OEO). The effectiveness of this new active packaging was checked for use in ready-to-eat salads. A plasticising effect was observed when OEO was incorporated in PLA films. The rest of the mechanical and physical properties of developed films did not show much change when OEO was included in the film. An antioxidant effect was recorded only for films containing the highest percentages of the active agent (5% and 10%). In addition, films exhibited in vitro antibacterial activity against Staphylococcus aureus, Yersinia enterocolitica, Listeria monocytogenes, Enterococcus faecalis and Staphylococcus carnosus. Moreover, in ready-to-eat salads, antimicrobial activity was only observed against yeast and moulds, where 5% and 10% of OEO was the most effective.


Assuntos
Antibacterianos/farmacologia , Antioxidantes/farmacologia , Embalagem de Alimentos , Óleos Voláteis/química , Óleos Voláteis/farmacologia , Origanum/química , Poliésteres/química , Antibacterianos/química , Antioxidantes/química , Enterococcus faecalis/efeitos dos fármacos , Listeria monocytogenes/efeitos dos fármacos , Testes de Sensibilidade Microbiana , Poliésteres/farmacologia , Staphylococcus/efeitos dos fármacos , Yersinia enterocolitica/efeitos dos fármacos
9.
Epilepsy Res ; 108(7): 1243-52, 2014 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-24908564

RESUMO

BACKGROUND: Eslicarbazepine acetate (ESL) is a new antiepileptic drug (AED) licensed as adjunctive therapy in adults with partial-onset or focal seizures. OBJECTIVE: To evaluate in a clinical practice setting the long-term efficacy and safety of ESL in patients with focal seizures. METHODS: ESLIBASE was a retrospective study that included all patients with focal seizures who started ESL between January 2010 and July 2012 at 12 hospitals. ESL was prescribed individually according to real-life practice. Efficacy and safety were evaluated over 1 year. Switching from carbamazepine (CBZ) and oxcarbazepine (OXC) was assessed. RESULTS: Three hundred and twenty-seven patients were included; 78% of patients were taking ≥2 other AEDs at baseline. Most (87%) began ESL because of poor seizure control and 13% because of adverse events (AEs) with CBZ or OXC. After 1 year, 237 patients (72.4%) remained on ESL. At 3, 6 and 12 months, the responder rate was 46.3%, 57.9%, and 52.5%, and 21.0%, 28.0%, and 25.3% of patients were seizure free. The responder rate significantly increased when ESL was combined with a non-sodium channel-targeting drug (non-SC drug) (66.7%) versus an SC drug (47.7%; p<0.001). At 12 months, 40.7% of patients had ≥1 AE; AEs led to treatment discontinuation in 16.2%. Dizziness, nausea, and somnolence were the most common AEs. The tolerability profile improved in >50% of the patients who switched from CBZ or OXC to ESL because of AEs. CONCLUSIONS: ESL was well tolerated and effective in a real-world setting over 1 year. Side-effect profile improved when OXC and CBZ recipients were switched to ESL.


Assuntos
Dibenzazepinas/uso terapêutico , Convulsões/tratamento farmacológico , Bloqueadores do Canal de Sódio Disparado por Voltagem/uso terapêutico , Adolescente , Adulto , Idoso , Idoso de 80 Anos ou mais , Feminino , Humanos , Estudos Longitudinais , Masculino , Pessoa de Meia-Idade , Estudos Retrospectivos , Estatísticas não Paramétricas , Fatores de Tempo , Adulto Jovem
10.
Anal Chim Acta ; 685(2): 204-11, 2011 Jan 31.
Artigo em Inglês | MEDLINE | ID: mdl-21168570

RESUMO

A fast HPLC method with diode-array absorbance detector and fluorescence detector for the analysis of 19 phenolic acids, flavan-3-ols, flavones, flavonols and caffeine in different types of samples was developed. Using a C(18) reverse-phase fused-core column separation of all compounds was achieved in less than 5 min with an overall sample-to-sample time of 10 min. Evaluation of chromatographic performance revealed excellent reproducibility, resolution, selectivity and peak symmetry. Limits of detection for all analyzed compounds ranged from 0.5 to 211 µg L(-1), while limits of quantitation ranged between 1.5 and 704 µg L(-1). The developed method was used for the determination of analytes present in different samples, including teas (black, white, green), mate, coffee, cola soft drink and an energetic drink. Concentration of the analyzed compounds occurring in the samples ranged from 0.4 to 314 mg L(-1). Caffeine was the analyte found in higher concentrations in all samples. Phytochemical profiles of the samples were consistent with those reported in the literature.


Assuntos
Bebidas/análise , Cafeína/análise , Cromatografia Líquida de Alta Pressão/métodos , Análise de Alimentos/métodos , Fenóis/análise , Cromatografia Líquida de Alta Pressão/instrumentação , Análise de Alimentos/instrumentação , Fenóis/química , Fatores de Tempo
11.
Talanta ; 82(5): 1986-94, 2010 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-20875606

RESUMO

The recent development of fused-core technology in HPLC columns is enabling faster and highly efficient separations. This technology was evaluated for the development of an fast analysis method for the most relevant soy isoflavones. A step-by-step strategy was used to optimize temperature (25-50°C), flow rate (1.2-2.7 mL/min), mobile phase composition and equilibration time (1-5 min). Optimized conditions provided a method for the separation of all isoflavones in less than 5.8 min and total analysis time (sample-to-sample) of 11.5 min. Evaluation of chromatographic performance revealed excellent reproducibility, resolution, selectivity, peak symmetry and low limits of detection and quantification levels. The use of a fused-core column allows highly efficient, sensitive, accurate and reproducible determination of isoflavones with an outstanding sample throughout and resolution. The developed method was validated with different soy samples with a total isoflavone concentration ranging from 1941.53 to 2460.84 µg g(-1) with the predominant isoflavones being isoflavone glucosides and malonyl derivatives.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Glycine max/química , Isoflavonas/análise , Cromatografia Líquida de Alta Pressão/instrumentação , Reprodutibilidade dos Testes , Proteínas de Soja/análise , Temperatura , Fatores de Tempo
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