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PubMed1991

[Solvent extraction-flow injection analysis for determination of trimethoprim in compound preparations].

Trimethoprim (TMP) in four pharmaceutical preparations (compound sulfamethoxazol tablets, compound tetracycline tablets, compound trimethoprim and sulfamethoxazol tablets; and compound berberine injection) is determined by solvent extraction-flow injection spectrophotometry. It can be extracted into chloroform directly, and the absorbance at a wavelength of 280 nm of the organic phase is measured after phase separation. The manifold comprises two streams. The sample is injected into a 0.2 mol/L NaOH carrier stream, and extracted with chloroform in a 200-cm coil (ID 0.7 mm) after a 50 cm reaction tube (ID 1.0 mm). Calibration graph is linear in the range of 25-150 micrograms/ml. The average recovery is 101.4% with a relative standard deviation of 1.1%. The proposed system permits the analysis of about 50 samples per hour. Precise results in agreement with those obtained with official methods are achieved.

Drug Combinations↗
PubMed2006

Determination of ceftriaxone sodium in pharmaceutical formulations by flow injection analysis with acid potassium permanganate chemiluminescence detection.

Based on the chemiluminescence (CL) emission generated from the oxidation of ceftriaxone sodium alkali hydrolysate by potassium permanganate in polyphosphoric acid (PPA), a novel determination method for ceftriaxone sodium was developed by using a flow-injection technique. The calibration curve appears to be linear in the range between 0.05 and 100 microg mL(-1) with a detection limit (3sigma) of 25 ng mL(-1), and a relative standard deviation (RSD) of 0.6% for eleven replicate determinations of 5.0 microg mL(-1) ceftriaxone sodium. The proposed method has been successfully utilized for the determination of ceftriaxone sodium in pharmaceutical formulations, while the chemiluminescence reaction mechanisms were investigated.

Calibration↗
PubMed1999

Improvement in the determination of mancozeb residues by the carbon disulfide evolution method using flow injection analysis.

The sample decomposition of the carbon disulfide evolution method for the determination of dithiocarbamate residues was carried out in a closed vial in the presence of hexane. The evolved carbon disulfide was extracted by the organic solvent and injected in a flow system for its quantification as copper complex. The conditions for batch decomposition, flow injection determination, and association of both were investigated with sodium diethyldithiocarbamate as model substance. An one-channel flow system was employed where the carrier stream was the ethanolic ethylenediamine/copper solution. The determination range was of 0. 01-1.26 microg of CS(2), with a relative standard deviation of 0.06% (n = 10), with a sample throughput of 45 samples/h. The association of the batch decomposition with the flow system was carried out with the fungicide mancozeb and was applied to the analysis of its residue in potato, lettuce, cucumber, and green bean crops. The approach allowed the analysis of 11 samples in triplicate in 2 h, with recoveries between 85% and 92% and relative standard deviation about 2%.

Carbon Disulfide↗
PubMed1999

Flow injection analysis of intracellular beta-galactosidase in Escherichia coli cultivations, using an on-line system including cell disruption, debris separation and immunochemical quantification.

A continuous integrated process for on-line quantification of intracellular components has been developed. By applying the concept of expanded micro-beds in a flow injection system it was possible to first perform on-line cell disintegration followed by an on-line binding assay for quantification of a reporter protein (beta-galactosidase) from the cell interior. The disintegration process involved the use of an expanded bed with immobilised lysozyme followed by ultrasonic treatment in a flow-through cell. The cell debris does not interfere in the binding assay as it is carried out in an expanded bed. The time for an assay cycle is at present approx. 35 min. This integrated system can be used for quantification of proteins down to at least 10(-7) mol/L.

Calibration↗
PubMedDate not supplied

Flow injection analysis of tetracyclines using inhibited Ru(bpy)3(2+)/tripropylamine electrochemiluminescence system.

Tetracyclines (TCs) were found to strongly inhibit the electrochemiluminescence (ECL) from the Ru(bpy)3(2+)-tripropylamine system when a working Pt electrode was maintained at 1.05 V (vs. Ag/AgCl) in pH 8.0 carbonate buffer solution. On this basis, a flow injection (FI) procedure with inhibited electrochemiluminescence detection has been developed for the determination of tetracycline (TC) and oxytetracycline (OTC). Under the optimized condition, the linear ranges of 2.0 x 10(-8)-1.0 x 10(-5) and 1.0 x 10(-8)-1.0 x 10(-5) g/mL and the detection limits of 4.0 x 10(-9) and 3.8 x 10(-9) g/mL were obtained for TC and OTC, respectively. The relative standard deviations (RSD) were 0.68% and 1.18% for 5.0 x 10(-7) g/mL TC and OTC (n = 13), respectively. The method showed higher sensitivity than most of the reported methods. It was successfully applied to the determination of tetracycline in a Chinese proprietary medicine, Tetracyclini and Cortisone Eye Ointment, and the residues of tetracycline in honey products. The inhibition mechanism has been proposed due to an energy transfer between electrogenerated Ru(bpy)3(2+)* and benzoquinone derivatives at the electrode surface.

Electrochemistry↗
PubMed2001

Tetracycline-selective electrode for content determination and dissolution studies of pharmaceuticals by flow-injection analysis (FIA).

The present work describes the construction and evaluation of different tetracycline (TC)-selective electrodes without inner reference solution and with polymer membranes. The several electrodes were prepared with poly(vinyl chloride) or ethylene(vinyl acetate) membranes comprising o-nitrophenyl octyl ether or bis(2-ethylhexyl)sebacate as mediator solvents and tetracycline tetrakis(4-clorophenyl)borate as ion exchanger. The best performance was recorded for the poly(vinyl chloride) membranes with bis(2-ethylhexyl)sebacate. Using solutions with adjusted ionic strength, this type of electrode presented a slope of 57.4 mV decade(-1) and a reproducibility of +/-0.3 mV day(-1), for an analytical range from 1.2 x 10(-4) to 1.0 x 10(-2) M. The pH working range was 2.0-3.8. Tubular-shaped potentiometric detectors based on the same selective membrane were also constructed. When TC solutions with adjusted ionic strength of concentrations ranging from 1.0 x 10(-4) to 1.0 x 10(-2) M were injected into a single-channel flow manifold, the detectors presented a slope of 56.6 mV decade(-1) and a reproducibility of +/-0.5 mV day(-1). The pH working range was 1.9-3.9. Both batch and flow procedures were applied to the potentiometric analysis of oral dosage forms. Average recoveries were within 98.6 to 100.3% and the t test indicated the accuracy of these results in comparison to an independent methodology. The flow system with the potentiometric detector was employed in dissolution studies as well.

Electrodes↗
PubMed2004

Successive determination of thiamine and ascorbic acid in pharmaceuticals by flow injection analysis.

A simple and rapid fluorimetric method for the determination of mixtures of thiamine and ascorbic acid is proposed. The procedure is based on the oxidation with mercury(II) of the B1 and C vitamins to form thiochrome (TC) and quinoxaline derivate, respectively. Both reaction products exhibit fluorescence at the same wavelengths (lambdaex = 356 and lambdaem = 440 nm). The procedure is optimised in a flow injection (FI) system and applied with excellent results in the determination of B1 and C vitamins in commercial pharmaceutical preparations. The calibration graphs were linear over the range 2-100 microg ml(-1) for thiamine and 5-100 microg ml(-1) for ascorbic acid. The throughput was 25 samples per hour.

Ascorbic Acid↗
PubMed2002

Evaluation of flow injection analysis for determination of urea in sheep's and cow's milk.

Difficulties in measuring the urea content in sheep's milk often occur with spectral photometry due to the high protein and fat concentrations of the milk. In this study an enzymatic flow procedure (QuickChem 8000 Ion Analyser, Lachat Instruments, Milwaukee, USA) to determine the urea content in ovine and bovine milk was evaluated. Urea content is determined by the Berthelot reaction after splitting it enzymatically with urease. The free ammonia diffuses through a teflon membrane into a stream of reagent solutions. Detection takes place by means of a reaction between the ammonium ions with hypochlorite and salicylate producing a green colour, which is measured spectrometrically in a flow meter at 660 nm. By using a diffusion cell chemical deproteinisation of milk is not necessary and capacity is high. The assessed procedure exhibited high accuracy and precision and reached a sample capacity of 55 samples an hour. Storage of the milk samples for several days as well as chemical preservation with bronopol had no effect on the measurement procedure. Due to the complexity of the apparatus and the costs associated therewith, the device proves less suitable for routine diagnostics but rather serves as a reference method for the measurement of urea concentration in milk.

Animals↗
PubMed2004

Simultaneous determination of levodopa and benserazide by stopped-flow injection analysis and three-way multivariate calibration of kinetic-spectrophotometric data.

The simultaneous determination of levodopa and benserazide in pharmaceutical formulations is described, based on the application of multidimensional partial least-squares regression to the kinetic-spectrophotometric data provided by diode-array detection within a stopped-flow injection method where analytes react with periodate. Flow injection parameters were adequately optimized. Accurate analysis is performed with no sample pre-treatment steps, and with minimum experimental effort. Satisfactory recovery results were obtained on a number of synthetic and commercial samples, in the latter case including the comparison with liquid chromatography measurements.

Benserazide↗
PubMed1980

Automated multiple flow-injection analysis in clinical chemistry: determination of total protein with Biuret reagent.

We have examined the feasibility of the automated multiple flow-injection technique for application to clinical chemistry by adapting to this system the biuret method for the determination of total protein. Samples were discretely and rapidly introduced into a continuously flowing, nonsegmented reagent stream by means of an automatic sampler and high-pressure injection valve. Pumps operating at 1380-2070 kPa (200-300 psi) were utilized to introduce the biuret reagent and saline diluent into the system separately at flow rates of 72 and 47 microL/s, respectively. Use of 20-microL sample and a 3.0-s reaction-delay coil was adequately sensitive for analysis for total protein by this method. Samples were analyzed at a rate of 150/h with no detectable between-sample carryover. Within-run precision studies yielded relative standard deviations of 2.5% and less. Total protein values obtained by this method correlated well with those obtained by centrifugal analyzer and bubble-segmented continuous-flow biuret methods.

Autoanalysis↗
PubMedDate not supplied

Principles and applications of flow injection analysis in biosensors.

In practical applications biosensors are often forced to operate under less than optimal conditions. Because of their construction, and the physical processes and chemical reactions involved in their operation, compromise conditions are frequently required to synchronize all events taking place. Therefore, and in order to implement functions such as periodic calibration, conditioning and possible regeneration of the biosensor, and, very importantly, to yield the freedom to select the optimum detection means, it is advantageous to use these devices in a flow-through mode, particularly by employing the flow injection (FI) approach. The capacity of FI, as offering itself as a complementary facility to augment the performance of biosensors, and in many cases as an attractive alternative, is demonstrated by reference to selected examples, comprising assays based on enzymatic procedures with optical and thermal detection procedures, and via description of a recently introduced technique for immunoassays, termed flow injection renewable surface immunoassays, which promises to entail powerful potentials and to yield compatible or better economy of operation than existing approaches.

Biosensing Techniques↗
PubMedDate not supplied

Chemiluminescence micro-flow-injection analysis on a chip.

Chemiluminescence microflow-injection analysis (microFIA) systems on a chip have been developed. The technology of laser ablation was used to fabricate the microchannels on the polymethyl methacrylate (PMMA) chip. The three sampling structure, including double-tee sampling structure, microvalve sampling structure and injection pump with accurate time control, were used. The microcolumn for specific molecular recognition, including molecularly imprinted polymer, enzyme and bacteria, were used to enhance selectivity. These microFIA systems have been applied to clinical analysis, assessment of food safety, in vivo and real-time determination of drugs, and pharmacokinetics studies.

Animals↗