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Biomedical subjects

A Gómez-Hens

Publications and source records attributed to A Gómez-Hens.

At least 19 recordsLinked to original sources
PubMed2006

Long-wavelength fluorimetry as an indirect detection system in immunoaffinity chromatography: application to environmental analysis.

The potential of long-wavelength fluorimetry when used as the detection system in immunoaffinity chromatography is assessed for the first time by applying this approach to the analysis of water and sludge samples. Nile blue (NB) was used to synthesize a long-wavelength fluorescent tracer for linear alkylbenzenesulfonates (LASs) using the carbodiimide method, in which the amino group of NB is covalently coupled to the activated carboxylic acid group of a LAS mimic with N-hydroxysuccinimide and dicyclohexylcarbodiimide. The method consists of the injection of a pre-incubated mixture containing linear sodium 4-dodecylbenzenesulfonate (LDS; used as the LAS model), anti-LAS antibodies, and the long-wavelength tracer into a commercial Protein G column. Free and bound tracer fractions are separated in the column, and the peak height of the immunochromatogram (corresponding to the free tracer) is directly measured at 626 nm (lambda (ex)) and 674 nm (lambda (em)), and then correlated to the analyte concentration. It is not necessary to perform an elution step immediately after every sample application. The dynamic range of the method is 0.05-2.5 microg ml(-1) LDS, and the detection limit is 15 ng ml(-1). The precision, expressed as the relative standard deviation, is 4.8-6.4%. Other surfactants (sodium dodecylsulfate and Triton X-100) do not cause interference. The recoveries obtained by applying the method to the analysis of water (ground- and wastewater) and sludge (primary and activated) samples ranged from 86.0 to 111.3%. Water sample analysis included an initial solid-phase extraction step, which cleaned up the samples and improved the detection limit fivefold.

Benzenesulfonates↗
PubMed2004

Selective kinetic determination of amikacin in serum using long-wavelength fluorimetry.

A simple and rapid method for the determination of the antibiotic amikacin, involving the use of a long-wavelength fluorophor, namely indocyanine green, (ICG) is presented. The dye is oxidised by cerium(IV) in acidic medium, resulting in a sharp decrease of the fluorescence, but this fluorescence quenching is inhibited in the presence of amikacin, which can be ascribed to the formation of an ion pair between the fluorophor and the analyte. The initial rate of the system is monitored at lambda(ex): 765 nm and lambda(em): 812 nm as excitation and emission wavelengths, respectively, using the stopped-flow mixing technique, which makes the method applicable to automatic routine analysis. Each measurement is obtained in only 2-3s. The method presents a detection limit of 0.02 microg m1(-1) in standard solutions, which corresponds to 2.5 microg ml(-1) in serum samples. The precision is in the range 4.8-6%. The good selectivity of the method allows amikacin to be determined in the presence of other antibiotics, including other aminoglycoside antibiotics, in serum. The recoveries obtained from the analysis of different samples were in the range 89.4-104.7%.

Amikacin↗
PubMed2000

Simultaneous stopped-flow determination of butylated hydroxyanisole and propyl gallate using a T-format luminescence spectrometer.

A simple and fast luminescent method is used for the first time to resolve a mixture of two synthetic antioxidants, propyl gallate (PG) and butylated hydroxyanisole (BHA), by the joint use of the stopped-flow mixing technique and a T-format luminescence spectrometer. The determination of these compounds involves two different and independent reactions. On the one hand, PG determination is based on an energy transfer process that involves the formation of a lanthanide chelate with terbium in the presence of Triton X-100 and tri-n-octylphosphine oxide. On the other hand, BHA is determined using a reaction between the oxidized form of Nile Blue and the antioxidant. Both systems are excited at the same excitation wavelength (310 nm), and the emission wavelengths are 545 and 665 nm for PG and BHA, respectively. The absence of overlap in the emission spectra makes it possible to measure separately the analytes in each channel of the instrument. Initial rate and equilibrium signal are used as analytical parameters and measured in 0.1 and 1 s for PG and BHA, respectively. Calibration graphs are linear over the range 0.09-3.5 microg mL(-)(1) for PG and 0.3-15 microg mL(-)(1) for BHA. The relative standard deviations of both systems are close to 2%. The proposed method is applied to the determination of these two antioxidants in several commercial food samples with recoveries ranging between 94.8 and 102.9% for PG and between 94.1 and 102.1% for BHA.

Butylated Hydroxyanisole↗
PubMed1999

Selective kinetic determination of paraquat using long-wavelength fluorescence detection.

The reaction between paraquat, ascorbic acid, and Cresyl Violet in alkaline medium and in the presence of sodium dodecyl sulfate has been applied for the first time to the development of a kinetic-fluorometric method for the determination of paraquat. The reaction rate of this system is measured by using the stopped-flow mixing technique, which makes the method applicable to automatic routine analysis. Analytical data are obtained in approximately 30 s. The calibration graph is linear over the range 6-500 ng mL(-)(1), and the detection limit is 1.8 ng mL(-)(1). The relative standard deviation is <3%. The use of dynamic measurements at long wavelength favors the high selectivity of the method. Diquat behaves in this system similarly to paraquat, but its interferent effect is easily avoided by using cysteine. The proposed method has been applied to the determination of paraquat in tap water, milk, and white wine samples with recoveries of 89-104%.

Animals↗
PubMed1999

Simultaneous determination of benzoic acid and saccharin in soft drinks by using lanthanide-sensitized luminescence.

A simple and fast approach is used for the first time to develop a time resolved lanthanide-sensitized luminescence method for the simultaneous determination of a preservative and a sweetener, namely benzoic acid (BZ) and saccharin (SC), respectively, in food samples. The method involves the formation of the corresponding ternary chelates with terbium(III) and trioctylphosphine oxide (TOPO) in the presence of Triton X-100, and the measurement of the initial rate and equilibrium signal of this system, which were obtained in 0.1 and 5 s, respectively. The dynamic ranges of the calibration graphs, obtained by using kinetic and equilibrium measurements, were 0.2-36 micrograms ml-1 and 0.15-30 micrograms ml-1, respectively, for BZ, and 3.3-24 micrograms ml-1 and 4-36 micrograms ml-1 for SC and the detection limits were 0.07 and 0.04 microgram ml-1, respectively, for BZ, and 1.1 and 1.2 micrograms ml-1, respectively, for sodium SC. The relative standard deviation ranged between 2.3 and 3.0%. Both compounds were determined simultaneously by using a system of two equations which were resolved by using the calibration data obtained individually for each analyte and by multiple linear regression. Mixtures of BZ and SC in ratios between 3:1 and 1:9 were satisfactorily resolved by using both approaches. The method was applied to the direct analysis of several soft drinks. Analytical recoveries ranged between 89.3 and 108.5%.

Benzoic Acid↗
PubMed1996

Advances in drug analysis by kinetic methods.

Automatic kinetic methods are powerful tools for drug analysis as they use modern instrumentation and computers, which are essential for shortening analysis times and enhancing the quality of routine analyses. This paper reviews novel kinetic approaches to the determination of various types of drugs in bio(pharmaceutical) materials including the following: (a) a combination of the stopped-flow (SF) technique and fluorescence polarization immunoassay for the determination of drugs of abuse and opiates in urine; (b) the joint use of the SF technique and micelle-stabilized room-temperature phosphorimetry for the determination of anti-inflammatory drugs such as naproxen; (c) the use of sensitized luminescence by energy transfer processes for the kinetic determination of antibiotics such as tetracycline using the SF technique; and (d) the use of the continuous addition of reagent technique for determining hallucinogenic alkaloids and phenothiazines by peroxyoxalate chemiluminescence reactions. Other advances in drug analysis by kinetic methods involving kinetometric approaches (e.g. Kalman filtering) and the use of micellar catalysis are also discussed.

Chemistry Techniques, Analytical↗
PubMed1996

Kinetic fluorimetric determination of gliadins in foods.

Kinetic methodology was applied for the first time to the determination of gliadin proteins by using a stopped-flow mixing technique. The method is based on two simultaneous processes: the reaction between gliadins and sodium dodecyl sulfate and the elimination of the quenching caused by this surfactant of the fluorescence of Cresyl Violet. Thus, the increase in fluorescence intensity with time is directly related to gliadin concentration. The use of this oxazine dye allows dynamic fluorescence measurements at long wavelengths, which avoids potential interferences from the sample matrix. The reaction rate is measured within 5 s, so the method is very suitable for the routine determination of gliadins in food samples. The dynamic range of the calibration graph was 0.5-50 micrograms ml-1 and the LOD was 0.25 microgram ml-1. The RSD was 1.6%. The method was applied to different food samples and the analytical recoveries were 88-107%.

Fluorometry↗
PubMed1995

Kinetic determination of nortriptyline in pharmaceutical samples by use of photometric and fluorimetric detection.

A fast kinetic method is proposed for the photometric and fluorimetric determination of nortriptyline hydrochloride. The method involves measuring the rate of formation of an adduct with 4-chloro-7-nitrobenzofurazan, which exhibits light absorption and fluorescent properties, and the use of a stopped-flow mixing technique, which facilitates application to automatic routine analyses. The reaction rate is measured within only 30 s. The detection limit is 0.12 micrograms ml-1 (photometry) and 0.18 micrograms ml-1 (fluorimetry) and the calibration graph is linear up to 60 micrograms ml-1 in both cases. The precision (as RSD) is less than 1.5%. The proposed method was satisfactorily used for direct analysis of pharmaceutical preparations and a mean recovery near 100% was obtained with both photometric and fluorimetric detection.

Hydrogen-Ion Concentration↗
PubMed1994

Direct stopped-flow fluorescence polarization immunoassay of abused drugs and their metabolites in urine.

Kinetic methodology was applied to the direct determination of abused drugs (amphetamines, cocaine, and cannabinoids) in urine by stopped-flow fluorescence polarization immunoassay (SF-FPIA). This technique provides analytical data within a few seconds by measuring the variation of polarized fluorescence with time during development of immunochemical reactions. Methods based on this principle are particularly suitable for routine screening of these drugs in urine, being more expeditious than conventional FPIA methods. The dynamic ranges of the calibration curves were 20-300 micrograms/L for d,l-amphetamine, 15-300 micrograms/L for benzoylecgonine (a cocaine metabolite), and 10-400 micrograms/L for 11-nor-delta 8-tetrahydrocannabinol-9-carboxylic acid (a cannabinoid metabolite). The detection limits and within- and between-assay precision were better than those provided by conventional FPIA. Analytical recoveries ranged between 97.5% for d,l-amphetamine and 102.4% for the cannabinoid metabolite. The results for the three analytes were consistent with those obtained by conventional FPIA.

Amphetamine↗
PubMed1993

Kinetic fluorimetric determination of promethazine by a stopped-flow mixing technique.

The oxidation of promethazine to its corresponding fluorescent sulphoxide was used to develop a novel kinetic fluorimetric method for the determination of this drug. The use of a stopped-flow mixing technique makes use of an oxidizing reagent unnecessary because the oxidation is rapidly carried out by dissolved oxygen. The method is simple and fast as it only requires a few seconds to obtain kinetic data which allows ready application to routine analyses. The calibration graph is linear over the range 0.5-80 micrograms ml-1 and the precision (%RSD) is close to 2%. The method was applied to the determination of promethazine hydrochloride in two pharmaceutical preparations.

Chemistry, Pharmaceutical↗
PubMed1993

Stopped-flow photometric determination of clavulanic acid in pharmaceutical and serum samples.

The stopped-flow mixing technique was used to develop a simple, fast kinetic method for the determination of clavulanic acid by reaction with imidazole. Whereas the conventional method requires about 12-15 min for equilibrium to be reached, kinetic measurements can be made within a few seconds. The calibration graph was linear over the range 1-40 microgram ml-1 of clavulanic acid and the detection limit achieved was 0.3 microgram ml-1. The precision and selectivity of the method are reported. The results obtained by applying the proposed method to the analysis of pharmaceutical and serum samples show how easily it can be adapted for routine analyses.

Clavulanic Acid↗
PubMed1989

Stopped-flow determination of procaine hydrochloride in pharmaceutical preparations.

A stopped-flow photometric method for the quantitative determination of procaine hydrochloride is proposed. It is based on the measurement of the rate of formation of a coloured product between procaine and sodium 1,2-naphthoquinone-4-sulphonate. The conversion of an equilibrium method to a kinetic method by the stopped-flow technique results in an improved detection limit and linear range, and in considerably increased sample throughput. A simple modular stopped-flow system has been used for this purpose. The results obtained on application of this method to the determination of procaine in various pharmaceutical preparations, show the suitability of the stopped-flow technique for routine pharmaceutical analyses.

Calibration↗
PubMed1989

A modular stopped-flow system for use in routine pharmaceutical analysis.

A modular stopped-flow system for routine pharmaceutical analysis is presented. It consists of an inexpensive stopped-flow module which is fitted to a spectrophotometer or spectrofluorimeter and controlled by a simple computer. The automatic technique developed with this system is suitable for the individual and simultaneous determination of various pharmaceuticals (anti-asthmatics, psychotropics, hormones, analgesics, anaesthetics and antiseptics) with satisfactory results.

Autoanalysis↗
PubMed1989

Stopped-flow determination of iodide in pharmaceutical and food samples.

The iodide-catalysed reaction between cerium(IV) and arsenic(III) has been studied using a modular stopped-flow system. The features of both the stopped-flow and conventional kinetic methods have been compared by using the same instrument. The stopped-flow method has a wider linear range and is faster than the conventional kinetic method and has been applied satisfactorily to the photometric determination of iodide in pharmaceutical preparations, table salt and cow's milk. The results obtained show that the stopped-flow method is simple, inexpensive and rapid and requires no sophisticated equipment. In addition, its high sampling rate makes it particularly suitable for the routine determination of iodide.

Food Analysis↗
PubMed1989

Stopped-flow--photometric and kinetic--fluorimetric methods for the determination of thyroid hormones in tablets.

The catalytic effect of thyroxine and triiodothyronine on the reaction between cerium(IV) and arsenic(III) was studied by using photometric and fluorimetric measurements. The kinetic - photometric studies were based on measurement of the decrease in absorbance of cerium(IV), whereas the rate of formation of fluorescent cerium(III) was measured in the kinetic - fluorimetric studies. A modular stopped-flow system was coupled to a spectrophotometer in order to develop stopped-flow methods for the determination of thyroxine and triiodothyronine. The proposed methods were compared and applied to the determination of these hormones in pharmaceutical preparations.

Kinetics↗
PubMed1989

Nonenzymatic stopped-flow fluorimetric method for direct determination of uric acid in serum and urine.

A simple, direct, sensitive, and selective stopped-flow method for the fluorimetric determination of uric acid in serum and urine samples is described. The variation of fluorescence intensity during the reaction between uric acid and 1,1,3-tricyano-2-amino-1-propene (triap) in the presence of hydrogen peroxide is monitored. For these kinetic measurements peroxide is monitored. For these kinetic measurements we used a versatile stopped-flow module that can be fitted to any fluorimeter. The linear range of the proposed method is 0.08-3.00 mg of uric acid per liter, and the detection limit is 0.03 mg/L. Within- and between-assay CVs and selectivity data are reported. Results for serum and urine samples correlated well with those obtained by the uricase method The proposed method is inexpensive and requires no sophisticated detection equipment.

Adult↗