999 resultados para SPE-HLLME-GS-MS


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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.

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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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An exhaustive classification of matrix effects occurring when a sample preparation is performed prior to liquid-chromatography coupled to mass spectrometry (LC-MS) analyses was proposed. A total of eight different situations were identified allowing the recognition of the matrix effect typology via the calculation of four recovery values. A set of 198 compounds was used to evaluate matrix effects after solid phase extraction (SPE) from plasma or urine samples prior to LC-ESI-MS analysis. Matrix effect identification was achieved for all compounds and classified through an organization chart. Only 17% of the tested compounds did not present significant matrix effects.

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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.

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Meropenem, a carbapenem antibiotic displaying a broad spectrum of antibacterial activity, is administered in Medical Intensive Care Unit to critically ill patients undergoing continuous veno-venous haemodiafiltration (CVVHDF). However, there are limited data available to substantial rational dosing decisions in this condition. In an attempt to refine our knowledge and propose a rationally designed dosage regimen, we have developed a HPLC method to determine meropenem after solid-phase extraction (SPE) of plasma and dialysate fluids obtained from patients under CVVHDF. The assay comprises the simultaneous measurement of meropenem's open-ring metabolite UK-1a, whose fate has never been studied in CVVHDF patients. The clean-up procedure involved a SPE on C18 cartridge. Matrix components were eliminated with phosphate buffer pH 7.4 followed by 15:85 MeOH-phosphate buffer pH 7.4. Meropenem and UK-1a were subsequently desorbed with MeOH. The eluates were evaporated under nitrogen at room temperature (RT) and reconstituted in phosphate buffer pH 7.4. Separation was performed at RT on a Nucleosil 100-5 microm C18 AB cartridge column (125 x 4 mm I.D.) equipped with a guard column (8 x 4 mm I.D.) with UV-DAD detection set at 208 nm. The mobile phase was 1 ml min(-1), using a step-wise gradient elution program: %MeOH/0.005 M tetrabutylammonium chloride pH 7.4; 10/90-50/50 in 27 min. Over the range of 5-100 microg ml(-1), the regression coefficient of the calibration curves (plasma and dialysate) were >0.998. The absolute extraction recoveries of meropenem and UK-1a in plasma and filtrate-dialysate were stable and ranged from 88-93 to 72-77% for meropenem, and from 95-104 to 75-82% for UK-1a. In plasma and filtrate-dialysate, respectively, the mean intra-assay precision was 4.1 and 2.6% for meropenem and 4.2 and 3.7% for UK-1a. The inter-assay variability was 2.8 and 3.6% for meropenem and 2.3 and 2.8% for UK-1a. The accuracy was satisfactory for both meropenem and UK-1a with deviation never exceeding 9.0% of the nominal concentrations. The stability of meropenem, studied in biological samples left at RT and at +4 degrees C, was satisfactory with < 5% degradation after 1.5 h in blood but reached 22% in filtrate-dialysate samples stored at RT for 8 h, precluding accurate measurements of meropenem excreted unchanged in the filtrate-dialysate left at RT during the CVVHDF procedure. The method reported here enables accurate measurements of meropenem in critically ill patients under CVVHDF, making dosage individualisation possible in such patients. The levels of the metabolite UK-1a encountered in this population of patients were higher than those observed in healthy volunteers but was similar to those observed in patients with renal impairment under hemodialysis.

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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.

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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.

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La LOCE i els decrets que la complementen estableixen que en el primer cicle de primària, els cursos en què s'aprèn a llegir i escriure, s'han impartir quatre hores setmanals de castellà. En aquest article s'analitzen les repercussions d¿aquesta mesura en el procés d'aprenentatge de la lectura i l'escriptura i en la consecució de l'objectiu lingüístic final del sistema educatiu a Catalunya (garantir el coneixement de les dues llengües oficials). La discussió gira entorn de tres eixos: la diversitat de coneixements lingüístics de l'alumnat que aprèn a llegir i escriure en una mateixa aula, la integració de l'ensenyament de la lectura i l'escriptura en les activitats que es desenvolupen al llarg de la jornada escolar, i la constatació que els infants aprenen a llegir i escriure en les llengües que fan servir els adults quan interaccionen amb ells, encara que els nens no les parlin correctament.

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Drug screening is an important issue in clinical and forensic toxicology. Gas chromatography coupled to mass spectrometry (GC-MS) remains the gold standard technique for the screening of unknown compounds in urine samples. However, this technique requires substantial sample preparation, which is time consuming. Moreover, some common drugs such as cannabis cannot be easily detected in urine using general procedures. In this work, a sample preparation protocol for treating 200 μL of urine in less than 30 min is described. The enzymatic hydrolysis of glucuro-conjugates was performed in 5 min thanks to the use of microwaves. The use of a deconvolution software allowed reducing the GC-MS run to 10 min, without impairing the quality of the compound identifications. Comparing the results from 139 authentic urine samples to those obtained using the current routine analysis indicated this method performed well. Moreover, additional 5-min GC-MS/MS programs are described, enabling a very sensitive target screening of 54 drugs, including THC-COOH or buprenorphine, without further sample preparation. These methods appeared as an interesting alternative to immuno-assays based screening. The analytical strategy presented in this article proved to be a promising approach for systematic toxicological analysis (STA) of drugs in urine.

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Fins on hem pogut esbrinar, el primer estudi publicat en una revista científica sobre la praderia o alguer de Posidonia oceanica de les illes Medes és el de De Haro (1965). En aquella època, la investigació delsfons marins estava als seus inicis i probablement la praderia de les illes Medes va ser un dels primers llocs en què, amb mitjans força precaris i a càrrec d’uns joves estudiants, es van efectuar prospeccions en immersió, tècnica que tot just començava però que molt ràpidament havia de substituir les dragues ialtres artefactes menys fiables. Amb el Programa de Bentos, entre 1972-1974 (Ros, 1982) –precisament aquest autor (vegeu el capítol 1) era un d’aquells «joves estudiants»; l’altre era en Jordi Camp, actualment investigador del CSIC–, la recerca bentònica va agafar un primer impuls i l’escafandre autònom es va incorporar plenament com a eina d’observació i mostreig. Durant aquest programa, es va situar una de les estacions de treball a les illes Medes, i l’alguer de Posidonia va ser un dels hàbitats objecte d’estudi, tot i que més aviat amb un objectiu faunístic i biocenòtic que estrictament ecològic.