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1.
Open Rheumatol J ; 3: 25-9, 2009 Jun 16.
Artigo em Inglês | MEDLINE | ID: mdl-19590596

RESUMO

OBJECTIVE: The study sought to ascertain the effectiveness of acupuncture as a treatment for fibromyalgia MATERIALS AND METHODS: THE FOLLOWING ELECTRONIC DATABASES WERE SEARCHED: PubMed; The Cochrane Library (CENTRAL); EMBASE; CINAHL; and Pascal Biomed (last date of search: January 2008). We analyzed pain intensity and patient withdrawals prior to termination of the study. A meta-analysis was performed, and a weighted global effect obtained using the inverse of variance. RESULTS: This review covered a total of 6 studies (323 subjects). No statistically significant differences were observed in terms of pain intensity (VAS): 0.02 (-0.24 a 0.28) or withdrawals: RR 0.91 (0.53 a 1.58) CONCLUSION: This systematic review found no evidence of benefit resulting from acupuncture versus placebo, as a treatment for fibromyalgia.

2.
Talanta ; 73(4): 742-7, 2007 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-19073096

RESUMO

A micropumping multicommutation manifold to perform turbidity determinations in waters is described. The procedure is based on the use of a combination of hydrazine sulfate and hexamethylenetetramine, to obtain an external standard of nephelometric turbidity units (NTU), which could compare the absorbance measurements at high wavelengths for samples with a calibration line obtained from a concentrated formazine standard diluted on-line. To minimize sample and reagent consumption and waste generation, the flow system was designed with two solenoid micro-pumps, one of them for the alternative introduction of the formazine standard and samples and the other one for the water carrier. The multicommutation approach makes possible the on-line dilution of a single standard to obtain the external calibration. The linear response was ranged up to 160NTU. The coefficient of variation was estimated as 1.6 and 3.2% for 10 and 100mm flow cell, respectively, for solutions containing 40NTU (n=10). Approximately, 60 determinations can be carried out per hour with limit of detection values of 1 and 0.1NTU, consuming only 160 or 240muL formazine solution and generating 1.8 or 2.0mL waste per determination, using measurement cells of 10 and 100mm optical pathlength, respectively. The procedure was successfully applied to 11 different water samples. Recovery studies were carried out and results obtained were between 97.5+/-0.2 and 100+/-1%. The development of a homebuilt light emitting diode (LED)-based portable flow analysis instrument was checked for in situ turbidimetric measurements, providing this equipment a LOD value of 0.09NTU working with a blue LED at 464nm and a LOD value of 0.1NTU working with an IR LED.

3.
J Autom Methods Manag Chem ; 2006: 20384, 2006.
Artigo em Inglês | MEDLINE | ID: mdl-17671614

RESUMO

A portable flow analysis instrument is described for in situ photometric measurements. This system is based on light-emitting diodes (LEDs) and a photodiode detector, coupled to a multipumping flow system. The whole equipment presents dimensions of 25 cm x 22 cm x 10 cm, weighs circa 3 kg, and costs 650 euro. System performance was evaluated for different chemistries without changing hardware configuration for determinations of (i) Fe(3+) with SCN(-), (ii) iodometric nitrite determination, (iii) phenol with sodium nitroprusside, and (iv) 1-naphthol-N-methylcarbamate (carbaryl) with p-aminophenol. The detection limits were estimated as 22, 60, 25, and 60 ng mL (-1) for iron, nitrite, phenol, and carbaryl at the 99.7% confidence level with RSD of 2.3, 1.0, 1.8, and 0.8%, respectively. Reagent and waste volumes were lower than those obtained by flow systems with continuous reagent addition. Sampling rates of 100, 110, 65, and 72 determinations per hour were achieved for iron, nitrite, phenol, and carbaryl determinations.

4.
Anal Bioanal Chem ; 383(1): 138-44, 2005 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-16094533

RESUMO

An automated and greener spectrophotometric procedure has been developed for the determination of phenol in water at 700 nm. The method uses the reaction between phenol, sodium nitroprusside, and hydroxylamine hydrochloride in a buffered medium at pH 12.3. The flow manifold comprises four solenoid micro-pumps employed for sample and reagent introduction into the reaction coil and to transport the colored product formed to the detector. The linear dynamic range was 50-3,500 ng mL(-1) (R = 0.99997; n = 6) and the method provided a limit of detection (3sigma) of 13 ng mL(-1). The sampling throughput was estimated to be 65 measurements per hour and the coefficient of variation was 0.5% (n = 10) for a 1.0 microg mL(-1) phenol concentration. Recoveries of 92-105% were obtained for phenol determination in spiked water samples at concentration levels from 50 to 5,000 ng mL(-1). The use of multicommutation reduced the reagent consumption 25-fold, the sample consumption 225-fold, and the waste generation 30-fold compared with the batch procedure. The proposed method is an environmentally friendly alternative to the official 4-aminoantipyrine method since it avoids the use of chloroform.


Assuntos
Fenóis/análise , Tecnologia Farmacêutica/métodos , Água/química , Ampirona/química , Autoanálise , Soluções Tampão , Concentração de Íons de Hidrogênio , Hidroxilamina/química , Nanotecnologia , Nitroprussiato/química , Espectrofotometria/métodos , Tecnologia Farmacêutica/instrumentação
5.
Talanta ; 66(3): 591-9, 2005 Apr 30.
Artigo em Inglês | MEDLINE | ID: mdl-18970025

RESUMO

It has been developed a fully mechanized procedure for the spectrophotometric determination of anionic surfactants in water expressed in terms of SDS concentration. The reference method, based on the reaction of SDS with methylene blue (MB) followed by extraction in chloroform, was mechanized in order to reduce the consumption of organic solvents. The system was based on the multicommutation approach and provided a 35 times reduction of the waste production without sacrificing the figures of merit of the method in terms of sensitivity and repeatability, for a dynamic linear range from 0.2 to 1.7mgl(-1). Results obtained for washing water samples were comparable with those obtained using the reference method and no significant differences, at 95% confidence level, were observed. Other useful characteristics are a solvent consumption of 0.7ml per determination, a sampling throughput of 40 determinations per hour, a relative standard deviation of 5.9% (n=10) for a sample containing 2x10(-6)moll(-1) (576mugl(-1)) surfactant and a limit of detection of 6.1x10(-9)moll(-1) (1.7mugl(-1)).

6.
Talanta ; 67(4): 673-7, 2005 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-18970223

RESUMO

A compact, reliable and low cost flow injection chemiluminescence system is described. The flow system consists of a set of solenoid micro-pumps that can dispense reproductive micro-volumes of solutions. The luminometer was based on a coiled cell constructed from polyethylene tubing that was sandwiched between two large area photodiodes. The whole equipment costs about US$ 750 and weights ca. 3 kg. Equipment performance was evaluated by measuring low concentrations of hydrogen peroxide by oxidation of luminol and for the determination of ammonium, based on its inhibition of the luminescence provided by the reaction of luminol and sodium hypochlorite. Linear responses were achieved within 1.0-80 micromol L(-1) H(2)O(2) and 0.6-60 micromol L(-1) NH(4)(+) with detection limits estimated as 400 nmol L(-1) H(2)O(2) and 60 nmol L(-1) NH(4)(+) at the 99.7% confidence level. Coefficients of variation were 1.0 and 1.8%, estimated for 20 micromol L(-1) H(2)O(2) and 15 micromol L(-1) NH(4)(+) (n=20), respectively. Reagent consumption of 55 microg luminol, effluent volume of 950 microL per determination and sampling rate of 120 samples per hour were also achieved.

7.
J AOAC Int ; 87(5): 1252-9, 2004.
Artigo em Inglês | MEDLINE | ID: mdl-15493684

RESUMO

A highly sensitive method was developed for determination of bismuth in milk shakes by multicommutation hydride generation atomic fluorescence spectrometry (HG-AFS) based on off-line sonication for 10 min with aqua regia 8% (v/v) and on-line waste treatment. The instrumentation and chemistry variables were studied in order to provide the best performance. The limit of detection in the original samples, established for a probability level of 99.6% (k = 3), was 1.67 ng/g Bi. The method provides a fast alternative in control analysis with a sampling throughput of 72 h as compared with 31 h obtained by the classical continuous measurement. Additionally, multicommutation reduces waste generation by a factor of 2.6. The consumption of sample, reductant, and blank, as compared with continuous mode HG-AFS, was reduced 9.6, 4.5, and 13.3 times, respectively. To confirm the accuracy of the method, recovery studies were performed, and excellent agreement between multicommutation and continuous measurement-based values was obtained. Application of the developed methodology for bismuth determination in milk shake samples from the Spanish market provided concentrations ranging from 4.2 to 15.0 ng/mL, and good comparability with data obtained by continuous measurements after microwave-assisted total digestion of samples for a 95% probability level and 12 degrees of freedom was found.


Assuntos
Bismuto/análise , Leite/química , Animais , Bovinos , Micro-Ondas , Espectrometria de Fluorescência , Espectrofotometria Atômica
8.
Anal Bioanal Chem ; 379(1): 83-9, 2004 May.
Artigo em Inglês | MEDLINE | ID: mdl-14740136

RESUMO

The aim of this study is to show the advantages of the emerging multicommutation methodology based on the use of solenoid valves for Te determination in milk by hydride generation atomic fluorescence spectrometry (HG-AFS). The delivery of a series of alternating sequential insertions of small volumes of samples and reagents gives rise to new hydrodynamic processes and exciting analytical potentials by controlling the time of flow through the on/off-switched solenoid valves. This drastically reduces the reagent consumption by a factor of 4 and the generation of effluents (590 mL h(-1) instead of 750 mL h(-1) generated by the continuous-mode measurement) and also provides an improvement in the laboratory productivity by an increase of the sample throughput (85 h(-1) compared to 20 h(-1) found in the continuous mode). So, multicommutation is an environmentally and economically sustainable alternative to the methodology based on continuous measurements. The multicommutation-based method developed was applied to tellurium determination in commercially available milk samples; a calibration range of 0.0-0.5 ng mL(-1) and a detection limit of 0.20 ng L(-1) with average relative standard deviation of 2.1% were found. Comparable results were obtained for a series of samples using both continuous and multicommutation HG-AFS modes.


Assuntos
Hidrogênio , Leite/química , Espectrofotometria Atômica/métodos , Telúrio/análise , Animais , Calibragem , Micro-Ondas , Análise de Regressão , Sonicação , Espectrofotometria Atômica/instrumentação , Fatores de Tempo
9.
Talanta ; 60(4): 809-19, 2003 Jul 04.
Artigo em Inglês | MEDLINE | ID: mdl-18969105

RESUMO

A multicommutation-based method has been developed for the on-line direct atomic fluorescence spectrometric (AFS) determination of Hg in waters without any previous sample treatment. The performance of the proposed procedure has been compared with that of a conventional AFS system based on continuous mode measurements. In short, the use of multicommutation, together with a reduction of the size of the liquid-gas phase separator, provides an increase of the laboratory productivity by improving the sample throughput by a factor of 3.6 and strongly reduces the sample consumed by a factor of 6 and reagent consumed by a factor of 8.4. The waste generation is reduced by a factor of 2.4 and the Ar consumed by a factor of 6, thus the developed method is an environmentally and economically sustainable alternative to the methodology based on continuous measurements, without any reduction of the analytical sensitivity and with an enhancement of the repeatability of measurements. Only the limit of detection was poorer for the methodology developed (1.3 ngl(-1)) than that found by the classical continuous mode (0.3 ngl(-1)). The aforementioned methodologies were applied to the determination of Hg in water samples having obtained comparable values by both procedures and with those found by an external laboratory.

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