1000 resultados para SBSE-HLLME-GS-MS
Resumo:
CE is a powerful analytical tool used to separate intact biomolecules such as proteins. The coupling of CE with TOF/MS produces a very promising method that can be used to detect and identify proteins in different matrices. This paper describes an efficient, rapid, and simple CE-ESI-TOF/MS procedure for the analysis of endogenous human growth hormone and recombinant human growth hormone without sample preparation. Operational factors were optimized using an experimental design, and the method was successfully applied to distinguish human growth hormone and recombinant human growth hormone in unknown samples.
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To study the stress-induced effects caused by wounding under a new perspective, a metabolomic strategy based on HPLC-MS has been devised for the model plant Arabidopsis thaliana. To detect induced metabolites and precisely localise these compounds among the numerous constitutive metabolites, HPLC-MS analyses were performed in a two-step strategy. In a first step, rapid direct TOF-MS measurements of the crude leaf extract were performed with a ballistic gradient on a short LC-column. The HPLC-MS data were investigated by multivariate analysis as total mass spectra (TMS). Principal components analysis (PCA) and hierarchical cluster analysis (HCA) on principal coordinates were combined for data treatment. PCA and HCA demonstrated a clear clustering of plant specimens selecting the highest discriminating ions given by the complete data analysis, leading to the specific detection of discrete-induced ions (m/z values). Furthermore, pool constitution with plants of homogeneous behaviour was achieved for confirmatory analysis. In this second step, long high-resolution LC profilings on an UPLC-TOF-MS system were used on pooled samples. This allowed to precisely localise the putative biological marker induced by wounding and by specific extraction of accurate m/z values detected in the screening procedure with the TMS spectra.
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La discusión sobre la eutanasia continúa siendo una de las más candentes en el ámbito de la bioética. En este artículo, analizaremos el debate entre quienes rechazan la eutanasia amparándose en la santidad de la vida humana y quienes la defienden propugnando como ideas fundamentales la calidad de vida y la autonomía individual. Tras estas visiones enfrentadas, subyace una discusión más profunda entre una concepción antigua de los derechos humanos, basada en el respeto a un orden «natural» y una concepción moderna de los mismos, heredera de un humanismo laico, que considera la autonomía el principal valor.
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"XVIII Congreso Internacional de Conservación y Restauración de Bienes Culturales - 18th International Meeting on Heritage Conservation", Granada 9 al 11 novembre de 2011
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M'han sol-licitat una breu presentació del treball que realitzem al grup 1 més 0, que jo coordino. Tractaré de resumir-ne les línies d'investigació en la brevetat de l'espai que m'han destinat. Com que el treball que es presenta és obra de diverses persones, hem inclas les seves adreces electròniques com a referéncies.
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Esta colaboración es una adaptación, escasamente actualizada, de la intervención en la Conferencia Diálogo del jueves 26 de noviembre de 2009, que bajo el título Hacia una sociedad inclusiva: los últimos 25 años de la educación social, se celebró dentro del 1º Congreso Catalán de la Educación Social, celebrado en Vic del 26 al 28 de noviembre de 2009. A pesar de los dos años y medio pasados, creo que no ha perdido actualidad. Es más, creo que algunas de las propuestas son ahora más urgentes que nunca.
Resumo:
Resulta evidente la necesidad de establecer mecanismos que permitan una descripción más exhaustiva de los recursos electrónicos. En este trabajo se propone como solución el uso de metadatos. Por ese motivo se estudia el concepto de metadato con el fin de determinar tanto su campo de acción como los diferentes presupuestos subyacentes en este.
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La población envejece progresivamente,lo que conlleva a un aumento de las patologías y de la demanda asistencial. En las Áreas Básicas de Salud, como el CAPs Eixample (ICS) de Barcelona, existe una demanda para mejorar el estado de salud y el bienestar de la población anciana, y la necesidad de encontrar innovaciones para hacer más eficiente la Asistencia sanitaria, hemos iniciado un proyecto de investigación y desarrollo para incrementar el bien estar, disminuyendo la morbilidad, y mejorando la calidad de vida de los ancianos. En este trabajo se describe el proyecto de Fisioterapia realizado en un marco multidisciplinario de profesionales de la sanidad.
Resumo:
The new-generation nebulizers are commonly used for the administration of salbutamol in mechanically ventilated patients. The different modes of administration and new devices have not been compared. We developed a liquid chromatography-tandem mass spectrometry method for the determination of concentrations as low as 0.05 ng/mL of salbutamol, corresponding to the desired plasma concentration after inhalation. Salbutamol quantification was performed by reverse-phase HPLC. Analyte quantification was performed by electrospray ionization-triple quadrupole mass spectrometry using selected reaction monitoring detection ESI in the positive mode. The method was validated over concentrations ranging from 0.05 to 100 ng/mL in plasma and from 0.18 to 135 ng/mL in urine. The method is precise, with mean inter-day coefficient of variation (CV%) within 3.1-8.3% in plasma and 1.3-3.9% in urine, as well as accurate. The proposed method was found to reach the required sensitivity for the evaluation of different nebulizers as well as nebulization modes. The present assay was applied to examine whether salbutamol urine levels, normalized with the creatinine levels, correlated with the plasma concentrations. A suitable, convenient and noninvasive method of monitoring patients receiving salbutamol by mechanical ventilation could be implemented. Copyright © 2011 John Wiley & Sons, Ltd.
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O objetivo do presente estudo foi avaliar os efeitos de diferentes dosagens de cloreto de mepiquat, thidiazuron e ethephon, aplicadas parceladamente no algodoeiro (Gossypium hirsutum L.) na Fazenda Itamarati, Ponta Porã, MS. As dosagens de cloreto de mepiquat foram: (0; 12,5 + 12,5 + 25,0 = 50; 25 + 25 + 25 = 75; 0 + 50 + 50 = 100; 12,5 + 62,5 + 50 = 125) g ha-1, com aplicações efetuadas aos 34, 47 e 62 dias após a emergência (DAE) em 1993/94, e aos 42, 60 e 73 DAE, em 1994/95, enquanto o thidiazuron foi aplicado quando 70% dos capulhos estavam abertos, nas dosagens de 0, 45, 60 e 75 g ha-1; já o ethephon foi aplicado sete dias após o thidiazuron, quando já se observava desfolha de 85%, nas dosagens de 0, 960 e 1.440 g ha-1. O delineamento experimental utilizado foi o de blocos casualizados em faixa, com subparcelas subdivididas e quatro repetições. O cloreto de mepiquat proporcionou redução do número de frutos verdes, aumento do peso de 100 sementes e do peso médio de um capulho; a percentagem de desfolha aumentou com as dosagens de thidiazuron e ethephon; constatou-se que a interação cloreto de mepiquat x thidiazuron x ethephon foi significativa para percentagem de abertura de capulhos e produção de algodão em caroço.
Resumo:
In addition to the importance of sample preparation and extract separation, MS detection is a key factor in the sensitive quantification of large undigested peptides. In this article, a linear ion trap MS (LIT-MS) and a triple quadrupole MS (TQ-MS) have been compared in the detection of large peptides at subnanomolar concentrations. Natural brain natriuretic peptide, C-peptide, substance P and D-Junk-inhibitor peptide, a full D-amino acid therapeutic peptide, were chosen. They were detected by ESI and simultaneous MS(1) and MS(2) acquisitions. With direct peptide infusion, MS(2) spectra revealed that fragmentation was peptide dependent, milder on the LIT-MS and required high collision energies on the TQ-MS to obtain high-intensity product ions. Peptide adsorption on surfaces was overcome and peptide dilutions ranging from 0.1 to 25 nM were injected onto an ultra high-pressure LC system with a 1 mm id analytical column and coupled with the MS instruments. No difference was observed between the two instruments when recording in LC-MS(1) acquisitions. However, in LC-MS(2) acquisitions, a better sensitivity in the detection of large peptides was observed with the LIT-MS. Indeed, with the three longer peptides, the typical fragmentation in the TQ-MS resulted in a dramatic loss of sensitivity (> or = 10x).
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Raltegravir (RAL), maraviroc (MVC), darunavir (DRV), and etravirine (ETV) are new antiretroviral agents with significant potential for drug interactions. This work describes a sensitive and accurate liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of plasma drug levels. Single-step extraction of RAL, MVC, DRV, ETV and RTV from plasma (100 microl) is performed by protein precipitation using 600 microl of acetonitrile, after the addition of 100 microl darunavir-d(9) (DRV-d(9)) at 1000 ng/ml in MeOH/H(2)O 50/50 as internal standard (I.S.). The mixture is vortexed, sonicated for 10 min, vortex-mixed again and centrifuged. An aliquot of supernatant (150 microl) is diluted 1:1 with a mixture of 20 mM ammonium acetate/MeOH 40/60 and 10 microl is injected onto a 2.1 x 50 mm Waters Atlantis-dC18 3 microm analytical column. Chromatographic separations are performed using a gradient program with 2 mM ammonium acetate containing 0.1% formic acid and acetonitrile with 0.1% formic acid. Analytes quantification is performed by electrospray ionisation-triple quadrupole mass spectrometry using the selected reaction monitoring detection in the positive mode. The method has been validated over the clinically relevant concentrations ranging from 12.5 to 5000 ng/ml, 2.5 to 1000 ng/ml, 25 to 10,000 ng/ml, 10 to 4000 ng/ml, and 5 to 2000 ng/ml for RAL, MRV, DRV, ETV and RTV, respectively. The extraction recovery for all antiretroviral drugs is always above 91%. The method is precise, with mean inter-day CV% within 5.1-9.8%, and accurate (range of inter-day deviation from nominal values -3.3 to +5.1%). In addition our method enables the simultaneous assessment of raltegravir-glucuronide. This is the first analytical method allowing the simultaneous assay of antiretroviral agents targeted to four different steps of HIV replication. The proposed method is suitable for the Therapeutic Drug Monitoring Service of these new regimen combinations administered as salvage therapy to patients having experienced treatment failure, and for whom exposure, tolerance and adherence assessments are critical.