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Biomedical subjects

Miguel Valcárcel

Publications and source records attributed to Miguel Valcárcel.

31 records · Page 2Linked to original sources
PubMed2004

Analytical potential of enzyme-coated capillary reactors in capillary zone electrophoresis.

Enzymes immobilized on the inner surface of an electrophoretic capillary were used to increase sensitivity and resolution in capillary zone electrophoresis (CZE). Sensitivity is enhanced by inserting a piece of capillary containing the immobilized enzyme into the main capillary, located before the detector, in order to transform the analyte into a product with a higher absorptivity. This approach was used to determine ethanol. In order to improve resolution, capillary pieces containing immobilized enzymes were inserted at various strategic positions along the electrophoretic capillary. On reaching the enzyme, the analyte was converted into a product with a high electrophoretic mobility, the migration time for which was a function of the position of the enzyme reactor. This approach was applied to the separation and determination of acetaldehyde and pyruvate. Finally, the proposed method was validated with the determination of ethanol, acetaldehyde, and pyruvate in beer and wine samples.

Alcohol Dehydrogenase↗
PubMed2004

Rapid determination of aliphatic amines in water samples by pressure-assisted monolithic octadecylsilica capillary electrochromatography-mass spectrometry.

A pressure-assisted capillary chromatography-mass spectrometry method based on the use of a monolithic octadecylsilica (ODS) capillary is proposed for the determination of aliphatic amines. A 25 mM citric acid buffer containing 10% methanol is used as running electrolyte. Separation is achieved by simultaneously applying a capillary electrophoresis (CE) voltage of 13 kV and an overimposed pressure of 8 bar. The use of pressure is required to ensure stable electrospray conditions. Analysis times are reduced by using a capillary column consisting of a 30 cm long monolithic silica capillary column bound with ODS and a fused-silica capillary column also 30 cm long. The proposed method was successfully applied to the determination of low-molecular-weight aliphatic amines in tap and river water. The analysis of real samples requires cleanup and preconcentration, which can be performed automatically by inserting a minicolumn in the replenishment system of the commercial instrument.

Amines↗
PubMed2004

Direct automatic determination of biogenic amines in wine by flow injection-capillary electrophoresis-mass spectrometry.

A capillary electrophoresis-electrospray mass spectrometry (CE-ESI-MS) method for the separation and determination of nine biogenic amines is proposed. Operational variables, such as the voltage, temperature, sheath liquid composition, flow-rate, and MS parameters, were optimized. Samples are injected in the hydrodynamic mode into a 75 cm x 50 microm ID coated capillary and separated by using 25 mM citric acid at pH 2.0. Heptylamine is used as internal standard. The experimental setup includes a flow manifold coupled to the CE system for automatic insertion of samples into the CE vials. The proposed method allows amines to be determined with limits of detection from 0.018 to 0.09 microg x mL(-1) and relative standard deviation (RSD) values from 2.4% to 5.0% (except 6.8% for histamine). The method was successfully used to determine biogenic amines in red and white wines.

Biogenic Amines↗
PubMed2003

Direct screening of lyophilised biological fluids for bile acids using an evaporative light scattering detector.

The usefulness of lyophilisation for the direct screening of biological fluids for bile acids was investigated. Human serum and urine were lyophilised without losses of the target compounds and further extracted with n-hexane in acidic medium under magnetic stirring. An integrated flow injection-liquid chromatographic system coupled to an evaporative light scattering detector (ELSD) was used for automated screening/confirmation. The continuous module allows sequential filtration of the organic phase, solvent changeover and solid-phase extraction for clean-up and preconcentration purposes. Retained bile acids were eluted with an acetonitrile-methanol (65:35, v/v) stream. For screening purposes, the effluent was directly introduced in the ELSD detector and the total bile acid content of the sample determined. For confirmatory analysis, another aliquot of the sample was processed in the screening module but the effluent was directed to the chromatographic columns, which provided the free bile acid profile of the sample. Fasting serum and urine samples obtained from healthy individuals were lyophilised and processed. Good agreement was obtained in the analysis of the two matrices assayed following the screening and confirmatory methods.

Bile Acids and Salts↗
PubMed2003

Liquid chromatographic determination of natural and synthetic colorants in lyophilized foods using an automatic solid-phase extraction system.

Five synthetic and five natural colorants were determined in lyophilized dairy products and fatty foods using an automatic method based on lixiviation and a solid-phase extraction process that includes cotton and RP-C(18) columns for the sequential retention of synthetic colorants and natural colorants, respectively. The lyophilization of the sample coupled with the separation procedure provides clean extracts despite the complexity of the matrices studied. In addition, the lyophilization process preserves the sample for at least 2 months without changes in the concentrations of the colorants. Identification and determination of synthetic and natural colorants were carried out using a liquid chromatograph equipped with a diode array detector. The detection limits achieved for all of the colorants (0.03-75 microg/g of lyophilized sample) allowed their determination within the limits established by the European Union, with good precision (approximately 4.5%). In addition, colorants spiked to different foods provided average recoveries (spiked at three concentration levels in four types of dairy samples and in three types of fatty foods) near 94 +/- 4%.

Autoanalysis↗
PubMed2003

Autoanalyzer for milk quality control based on the lactose, fat, and total protein contents.

A novel autoanalyzer was developed to assess the quality of milk samples according to the percentage of lactose, fat, and total protein they contain. The module comprises two pumps (one of high pressure), an injection valve, a filter, and an evaporative light-scattering detector. A volume of 15 microL of dilute milk was injected in an ethanol-water (50% v/v) stream for precipitation/retention of protein/fat, being the lactose content determined in the filtrate. The fat fraction was calculated using an ethanol stream, and total protein was finally dissolved by means of a 1.7 mol/L acetic acid solution. The simplicity of the proposed automatic module lies in the universal response of the detector, which permits the determination of the three macrocomponents in milk. In addition, the flow injection method allows their sequential analysis in the same injected sample by using selective reagents for each compound. The proposed method was validated with an SRM milk sample as well as by comparison of the results obtained with those provided by the IR method. In addition, the proposed analyzer is cheaper than its counterpart that is based on infrared technique.

Animals↗
PubMed2003

Determination of natural and synthetic colorants in prescreened dairy samples using liquid chromatography-diode array detection.

A simple and novel screening method for food colorants was proposed. Synthetic or natural colorants were discriminated as they were selectively adsorbed on cotton or RP-C18 sorbent columns, respectively. After elution, each fraction was monitored at 400, 530, and 610 nm for yellow, red, and green-blue-brown additives, respectively, with a DAD spectrophotometer. The screening method serves as a filter to indicate whether the target colorants are present above or below the detection limit of the method (6-15 or 25-10,000 n/mL for synthetic or natural colorants, respectively). Positive samples were discriminated by LC-DAD, using a flow system similar to that of the screening method. The LC-DAD discrimination/confirmation method is very sensitive; it exhibits a linear range of 0.01-50 microg/mL (excluding curcumin and caramel, which are linear up to 200 and 1,500 microg/mL, respectively). The method was applied to the determination of natural and synthetic colorants in dairy samples with good precision.

Animals↗
PubMed2003

Determination of nitrosamines in preserved sausages by solid-phase extraction-micellar electrokinetic chromatography.

A new methodology for extraction, pre-concentration and analysis of nitrosamines in meat derived products was developed. The samples (canned sausages) were distilled in vacuum steam and the nitrosamines were pre-concentrated by solid-phase extraction with active carbon. Then, micellar electrokinetic chromatography was used for the separation and determination of the different nitrosamines contained in a real sample and gas chromatography with mass spectrometry detection was used as the confirmation technique. The method allowed the determination of nitrosamine compounds at trace levels with relative standard deviation ranging from 4.0 to 22%.

Animals↗
PubMed2003

Determination of myo-inositol phosphates in food samples by flow injection-capillary zone electrophoresis.

A capillary electrophoresis (CE) method with indirect photometric detection was developed to identify and quantify myo-inositol phosphates in food samples. A flow-injection (FI) system including a micro-column containing anionic exchange resin was used for the solid-phase extraction of the myo-inositol phosphates with a view to their preconcentration. The FI system was automatically coupled to CE equipment via a mechanical interface. The overall analysis time was shortened by incorporating an FI system for myo-inositol hexakisphosphate monitoring. The limit of detection for myo-inositol phosphates as determined by FI-CE ranged from 11 to 26 micromol/L and the coefficient of variation from 3.9 to 5.0%. On the other hand, the limit of detection and coefficient of variation for myo-inositol hexakisphosphate as monitored by the FI system were 75 micromol/L and 2.9%, respectively. The proposed method was successfully applied to a variety of food samples with recoveries ranging from 96.0 to 107.7% and the precision from 3.9 to 7.9%. Based on the results, the content of myo-inositol hexakisphosphate in nuts was two or three times higher than that in legumes.

Electrophoresis, Capillary↗
PubMed2003

Development of a new method for the determination of nitrosamines by micellar electrokinetic capillary chromatography.

A new method was developed for separation and quantification of nitrosamines by micellar electrokinetic capillary chromatography (MEKC). The effects of composition of the buffer, concentration of sodium dodecyl sulfate (SDS), gamma-cyclodextrin (CD) and pH on the separation and migration times of the nitrosamines were investigated. The different instrumental variables affecting sensitivity and resolution, such as power supply, injection mode and wavelength for measurement, were carefully optimized. The direct application of this method to aqueous synthetic samples allowed the separation and determination of nitrosamine mixtures at the mg x L(-1) level. The calibration curves revealed a linear range between 0.25 and 10 mg x L(-1), with detection limit (DL) varying from 0.16 to 0.27 mg x L(-1), quantification limit (QL) varying from 0.52 to 0.90 mg x L(-1), and RSD relative standard deviation (RSD) from 4.5% to 8.5%. The proposed method was successfully applied to the determination of dimethylnitrosamine (DMN), diethylnitrosamine (DEN), N-nitrosopyrrolidine (NPYR), N-nitrosomorpholine (NMOR) and N-nitrosopiperidine (NPIP).

Calibration↗
PubMed2002

Speciation of lead in environmental waters by preconcentration on a new fullerene derivative.

A novel fullerene derivative including a chelating group attached to the fullerene core has been prepared by photoreaction of C60 and sodium diethyldithiocarbamate (NaDDC) in toluene-methanol medium. The optimization of the synthesis procedure was monitored by UV-visible spectroscopy using the spectrum of C60 fullerene as reference; the new material, a C60-NaDDC monoadduct, showed a shoulder at 430 nm and an increase in the absorption band comprised between 425 and 500 nm. The solid was obtained by photolysis reaction in approximately 24 h, requiring further purification by preparative chromatography. Characterization of the brown product was accomplished by XRD and solid-state 13C MAS NMR; chemical modification was confirmed through the appearance of peaks close to the fullerene core peak located at 146.9 ppm, which can be assigned to carbon atoms of C60 that are covalently bonded to the diethyldithiocarbamate group to form a pyrrolidine ring-fused fullerene monoadduct. Using lead species as a model assessed the ability of the new material for the preconcentration of metallic and organometallic compounds, providing detection limits of 4-15 ng/L. The most interesting conclusions of the results were high adsorption efficiency, selectivity, and stability of the C60-NaDDC derivative (the packed material can be used for at least six months).

Fullerenes↗
PubMed2002

A method for screening total mercury in water using a flow injection system with piezoelectric detection.

An automatic microgravimetric screening system based on piezoelectric detection and the use of acidic stannous chloride as reductant was developed for the fast detection and determination of total mercury in water. Reduced mercury is detected as an amalgam by using a gold-coated piezoelectric crystal, the sensor subsequently being regenerated by passing it through a peroxydisulfate solution. The gold-coated piezoelectric crystal is a highly efficient retention unit for the main soluble mercury species (inorganic, complexed, and organometallic) previously reduced to elemental mercury and is free of interferences from other metal ions. This detector exhibits good sensitivity: it allows the determination of mercury at sub-parts-per-billion concentration levels (0.30-1.00 microg/L). The precision, expressed as relative standard deviation, was +/- 2.7% (n = 11; P = 0.05) at 0.5 microg/L total mercury. The proposed method was successfully used as a rapid screening method for mercury monitoring in natural waters.

Electrochemistry↗