Search PubMed⌕ Search

SEARCH · Search PubMed

Results for “Flow Injection Analysis”

Search indexed PubMed citations on genomics, clinical trials, systematic reviews and public health. Explore titles, authors and supplied subject terms, then open the PubMed record.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,567 records · Page 87Linked to original sources
PubMed2000

Selective determination of pyridoxine in the presence of hydrosoluble vitamins using a continuous-flow solid phase sensing device with UV detection.

A very simple, inexpensive and highly selective flow injection UV spectrophotometric method for the determination of vitamin B(6) is presented. The native absorbance of the analyte is continuously monitored at 290 nm when it is transiently retained on Sephadex SP C-25 cation exchanger gel beads placed in the detection area of a flow cell. The preconcentration on the active solid phase provides by itself a high increase in sensitivity compared with the same procedure carried out without a solid support. The analytical response is linear in the concentration ranges 1-10 and 2-20 microg ml(-1) using 600 and 1250 microl of sample, respectively. The R.S.D. (%) are 0.65 (600 microl) and 0.84 (1250 microl) and the detection limits 0.08 and 0.02 microg ml(-1), respectively. The procedure was successfully applied to the determination of vitamin B(6) in pharmaceuticals containing (among other active principles) hydrosoluble vitamins in much higher concentrations than that tolerated by the method if performed in aqueous solution. Nevertheless they were tolerated using the proposed sensor due to the selective retention of the analyte.

Ascorbic Acid↗
PubMed2001

Flow injection potentiometric determination of bismuth(III) in anti-acid formulations.

A flow injection potentiometric procedure is proposed for determining bismuth(III) in anti-acid formulations. In this work, a tubular electrode coated with an ion-pair formed between [Bi(EDTA)](-) and tricaprylylmethylammonium cation (Aliquat 336) in a poly(vinylchloride) (PVC) was constructed and used in a single channel flow injection system. The effect of membrane composition, pH and flow injection parameter over the Bi(III) tubular electrode response (slope (mV/decade)) was initially evaluated in quintuplicate in 0.5 mol l(-1) EDTA solution as carrier. The best response (-59.6+/-0.9 mV/decade) was attained with the 5% m/m ion-pair; 65% m/m o-nitrophenyl octyl ether (o-NPOE) and 30% m/m PVC in pH 6-9. The electrode showed a linear response to E (mV) versus log [Bi(EDTA)](-) in the bismuth(III) concentration range from 2.0x10(-5) to 1.0x10(-2) mol l(-1) and a useful lifetime of at least 5 months (more than 1000 determinations for each polymeric membrane). The detection limit was 1.2x10(-5) mol l(-1) and the R.S.D. was less than 2.0% for a solution containing 5.0x10(-4) mol l(-1) bismuth(III) (n=10). Several species such as Cd(II), Mn(II), Ni(II), Zn(II), Co(II), Cu(II), Mg(II), Cr(III) and Al(III) at 1.0x10(-3) mol l(-1) concentration in 0.5 mol l(-1) EDTA solution did not cause any interference. The frequency rate was 90 determinations per hour and the results obtained for bismuth(III) in anti-acid formulations using this flow procedure and those obtained using a spectrophotometric procedure are in agreement at the 95% confidence level.

Antacids↗
PubMed1999

Degradation study of thiotepa in aqueous solutions.

The degradation of N,N',N"-triethylenethiophosphoramide (thiotepa) in aqueous solutions has been investigated over the pH range 1-14. Samples were analyzed using a high-performance liquid chromatographic system with UV detection. The degradation kinetics were studied as a function of pH, sodium chloride concentration and temperature. The degradation of thiotepa follows pseudo first order kinetics. The pH-log kobs profile shows that thiotepa is most stable in the pH range 7-11. At pH?11 chloride has no influence on the degradation rate. The degradation products were isolated and the structures identified by mass spectrometry. Chloro adducts of thiotepa are generated in the presence of sodium chloride and in acidic medium. In the pH range 7-11 only the mono-chloro adduct of thiotepa could be found. No detectable degradation products were formed at pH?11.

Algorithms↗
PubMed2000

Automated flow-injection spectrophotometric determination of catecholamines (epinephrine and isoproterenol) in pharmaceutical formulations based on ferrous complex formation.

A novel automated flow-injection spectrophotometric method for the determination of catecholamines (epinephrine and isoproterenol) has been developed based on the formation of their coloured complexes with Fe(II) in aminoacetic-carbonate buffer pH 8.3 and measuring of the absorbance peaks at the lambda(max) of 530 nm. A fully automated FIA system controlled by home-made software (FIA-MOD) was used for optimising the chemical and manifold parameters and running of routine measurements. The calibration graph was linear in the range of 5-200 mg l(-1) for epinephrine with an RSD of 0.24% (n = 5; c = 150 mg l(-1)) and 10-300 mg(-1) for isoproterenol with an RSD of 0.13% (n = 5; c = 200 mg l(-1)). Measurement throughput was 120 h(-1) ensuring a sample throughput of 40 h(-1) analysed in triplicate. Common excipients for tablets and injections were found not interfering. The proposed method was applied for the assay of various commercial pharmaceutical formulations containing epinephrine and isoproterenol and for the content uniformity test for the isoproterenol tablets. The assay results with RSD 2-4% (n = 3) were comparable with those obtained with the official USP XXIII methods (mean difference 1.9%).

Artifacts↗
PubMed2001

Flow injection determination of levodopa in tablets using a solid-phase reactor containing lead(IV) dioxide immobilized.

A flow injection spectrophotometric procedure was developed for determining levodopa in tablets. The determination of this drug was carried out by reacting it with lead(IV) dioxide immobilized in polyester resin packed in a solid-phase reactor and the dopachrome yielded was monitored at 520 nm. The analytical curve for levodopa was linear in the concentration range from 1.0x10(-4) to 1.0x10(-3) mol l(-1) with a detection limit of 8.0x10(-5) mol l(-1). The relative standard deviation (R.S.D.) was 0.2% for a solution containing 4.0x10(-4) mol l(-1) levodopa (n=10), and 90 determinations per hour were obtained.

Flow Injection Analysis↗
PubMed2001

Simultaneous determination of thiamine and pyridoxine in pharmaceuticals by using a single flow-through biparameter sensor.

For the first time, an UV-photometric flow-through sensing device has been developed for the simultaneous determination of two cationic species (thiamine and pyridoxine). The sensor is based on the retention of the analytes on a cationic ion-exchanger gel placed in the detection zone itself into a quartz flow-cell. A double discrimination is used for detecting the analytes: (a) a double and simultaneous working wavelength, performed by the use of a diode array detector; and (b) a temporary sequentiation in the arrival of the analytes to the sensing zone by on line separation using a cationic ion-exchanger (the same used in the sensing zone) placed into a minicolumn just before the flow cell. Pyridoxine is determined the first (by measuring its intrinsic absorbance at 293 nm) because it passes through the minicolumn while thiamine is strongly retained on it. Then, thiamine is conveniently eluted from the precolumn and its intrinsic UV absorbance measured at 255 nm. In both cases, transitory signals were obtained because both the carrier (in the case of the pyridoxine) and the eluting (in the case of thiamine) solutions used also eluted the respective analyte from the sensing zone. Using 1000 microl of sample, the analytical signal showed a very good linearity in the range 2-30 microg ml(-1) for both analytes with detection limits of 0.10 and 0.084 microg ml(-1) for thiamine and pyridoxine, respectively. The optosensor was satisfactorily applied to the determination of these two analytes in pharmaceuticals.

Flow Injection Analysis↗
PubMed2001

Automatic multicommmutated flow system for diffusion studies of pharmaceuticals through artificial enteric membrane.

An automatic flow procedure with spectrophotometric detection was developed for the study of pharmaceuticals diffusion through an artificial enteric membrane. The manifold comprised two independent flow pathways, gathered by a diffusion unit with two compartments and an enteric lipophilic membrane. The pathways were automatically filled with solutions simulating digestive and plasmatic conditions by means of four solenoid valves. The diffusion of pharmaceuticals from the enteric to the plasmatic compartment was performed in closed loop pathways, and was continuously monitored by a flow cell coupled to the acceptor solution pathway. The volumes of the digestive and plasmatic solutions were 6.0 and 3.6 ml, respectively, which comprised filling unit compartment, pumping tubing and connecting flow lines. Pumping flow rates of donor and acceptor solutions were maintained at 6.0 and 2.5 ml min(-1), respectively. The proposed system was employed in diffusion studies of caffeine and aminophylline, and in the evaluation of the influence of tensioactive agents on the diffusion process. After continuous solutions circulation for 60 min, caffeine concentration in the acceptor stream was ca. 18% of its initial concentration at the digestive compartment. The system could be programmed to perform several replicates, stopping them with different degrees of diffusion without operator assistance. The data generated by the spectrophotometer was read by the microcomputer as a time function, and stored for further mathematical treatment.

Aminophylline↗
PubMed2001

Importance of injection solution composition for LC-MS-MS methods.

For the first time, the influence of the injection solution composition on the quality of LC-MS-MS methods, in terms of column efficiency and peak shape, was systematically investigated. Various types of compounds, including polar ionic acidic, polar ionic basic and non-polar neutral compounds, were prepared in different solutions ranging from 100% water to 100% acetonitrile. Different volumes of these solutions were injected onto either C18 or silica columns connected to tandem mass spectrometry. The mobile phases consisted of acetonitrile, water, and small amounts of volatile acid or buffer. On silica columns, the influence of injection solution on the peak shape and column efficiency was straightforward. The sharpest peaks and the highest column efficiency were obtained with 100% acetonitrile as the injection solvent. On C18 columns, this type of influence was less clear due to the dual retention mechanism of the bonded phase and of the residual silanol groups. On C18 column, retention due to residual silanol groups was significant even with a mobile phase containing less than 50% acetonitrile. Poor peak shape was observed when the injection solution had a stronger eluting strength than mobile phase, particularly for early eluting peaks.

Acetates↗
PubMed2001

Potential of on-line micro-LC immunochemical detection in the bioanalysis of cytokines.

An on-line liquid chromatography-immunochemical detection (LC-ICD) system for the quantification of cytokines in cell extracts has been developed using a post-column continuous-flow reaction detection system using fluorescence labelled antibodies. Cytokines eluting from the micro-HPLC column react with antibodies to form fluorescent complexes. In a second step the excess of free antibody is trapped on a cytokine bound support prior to fluorescence detection. The concentration detection limit of the flow injection-ICD system was 50 pM (20 microl injection volume) for interleukin 4 (IL-4). An absolute detection limit of 1 fmol was obtained for IL-4. Similar to ICD systems for small non-protein analytes developed earlier, reaction times were in the order of 1 minute. The immobilised cytokine affinity columns can easily be regenerated and used for months. The present ICD system for interleukins 4, 6, 8 and 10 was coupled to ion exchange-, size exclusion- and reversed phase chromatography. Important parameters (reaction times, reaction conditions) were investigated to get a better understanding of post-column ICD systems for macromolecules.

Chromatography, Gel↗
PubMed2001

Flow-injection extraction-spectrophotometric method for the determination of ranitidine in pharmaceutical preparations.

The spectrophotometric determination of trace amounts of ranitidine was carried out by liquid-liquid extraction using bromothymol blue with a flow system. The determination of ranitidine in the range of 1 x 10(-5) - 1 x 10(-4) mol l(-1) was possible with a sampling frequency of 40 samples h(-1). The method was satisfactorily applied to the determination of ranitidine in pharmaceutical preparations and the recovery was quantitative and no interferences from excipients were observed.

Anti-Ulcer Agents↗
PubMed2002

Simultaneous dissolution profiles of two drugs in pharmaceutical formulations by an FIA manifold.

This article deals with the simultaneous determination of dissolution profiles of two drugs with overlapped spectra, present in the same pharmaceutical formulation. The official procedure for the dissolution profile is adapted to the continuous-flow methodology; the dissolution vessel is connected to an FIA manifold, in which the sample aliquots from the dissolution vessel are treated in order to adjust to the suitable pH and dilution degree to be monitored. The resulting solution is injected into the carrier stream, an acetic acid-acetate buffer at pH 4.3 and forced to the flow-cell of the spectrophotometer. The simultaneous determination of both profiles is based on the first derivative spectra and the zero-crossing mathematical procedure. The empirical profile of the curve is adjusted by regression using different approaches; the three-parameter plot method is selected. The analytical errors, when the concentration of one drug is very low or very high, are also checked. A binary mixture in commercially available formulations of solid oral administration of sulphametoxazole and trimethoprim is presented.

Anti-Infective Agents↗
PubMed2002

Oxidation of adrenaline and noradrenaline by solved molecular oxygen in a FIA assembly.

A simple and effective procedure is proposed for the study and simultaneous determination of adrenaline and noradrenaline. The fluorimetric determination of both substances is performed in a flow injection assembly and by oxidation of both drugs with the solved molecular oxygen. The influence of different parameters is empirically studied and the interpretation of the reaction mechanism is also added. The determination of adrenaline is monitored at 450 nm and the outputs at 520 nm correspond to the adrenaline and noradrenaline global amount; for both lectures lambda(exc) 329 nm. The influence of temperature is relevant and analytical determination occurred at 55 degrees C by immersing the sample loop in a water bath. The linear range for adrenaline is over 0.5-20 microg ml(-1), limit of detection for both compounds is 0.2 microg ml(-1): the influence of foreign compounds as potential interferents is also tested; and, finally the procedure is applied to determination of both chatecolamines in synthetic samples.

Epinephrine↗
PubMed2002

Determination of zinc (II) in pharmaceuticals based on a flow-through bulk optode.

A method based on flow injection (FI), was applied for the determination of Zn (II) using a flow-through bulk optode membrane that incorporates 1-(2-pyridylazo)-2-naphthol in a plasticized poly (vinyl chloride) membrane entrapped in a cellulose support. The calibration graph plotting the reflectance at 562 nm versus [Zn (II)] was linear in the range 0.16-3.27 mgl(-1) (2.5 x 10(-6)-5 x 10(-5) M) with a detection limit of 0.10 mgl(-1). The variation coefficients of the sensor response for 0.33 mgl(-1) of Zn (II) were +/-0.11% for consecutive measurements (n=10), +/-0.19% between days (n=5) and +/-0.22% between different membranes (n=6). The sensor can be readily regenerated with the same acetic/acetate carrier of pH 3.9. The FI method proposed was applied to the determination of zinc (II) in pharmaceuticals.

Flow Injection Analysis↗
PubMed2002

Determination of diphenhydramine hydrochloride in some single tertiary alkylamine pharmaceutical preparations by flow injection spectrophotometry.

A simple and rapid spectrophotometric method with flow injection is proposed for determination of diphenhydramine hydrochloride in some single tertiary alkylamine pharmaceutical preparations (capsule and syrup). It is based on ion pair formation with bromocresol green in a pH 3 buffer which a yellow ion pair compound is extracted into chloroform layer. An aqueous layer containing excess bromocresol green is injected into a carrier stream of 0.01 M borax solution and absorbance of the stream is continuously monitored at 610 nm. Diminution of the bromocresol green is related to an amount of diphenhydramine hydrochloride that can be evaluated from a calibration graph established by a plot of diphenhydramine hydrochloride concentration (micro gm l(-1)) and peak height (mV). Optimization will be discussed. The calibration graph is linear over the concentration ranges of 5-21 and 75-188 micro gm l(-1). A throughput of 100 injections h(-1) can be obtained. Application to assay for capsule and syrup samples has been demonstrated. The method is validated by comparing the results with HPLC analyses.

Bromcresol Green↗
PubMed2002

Flow injection photochemical spectrofluorimetry for the determination of carbamazepine in pharmaceutical preparations.

Upon on-line photochemical reaction carbamazepine (CBZ) can be converted to a strong fluorescent compound which has a maximum emission wavelength of 478 nm and maximum excitation wavelength of 254 nm. Acidity of reaction medium and the acid type were found to be critical for the on-line photochemically induced fluorescence, dilute hydrochloric acid being the most suitable. Based on these observations, a flow injection photochemical spectrofluorimetric approach for determination of the drug was developed. At optimized conditions, a detection limit of 0.08 ng x ml(-1) CBZ was achieved at the sampling rate of 80 h(-1). Eleven determinations of a 100 ng ml(-1) CBZ standard solution gave a RSD of 0.45%. A linear calibration curve was obtained in the CBZ concentration range of 2-250 ng x ml(-1). The developed method was successfully applied to assay the CBZ contents in pharmaceutical tablets.

Carbamazepine↗
PubMed2002

Flow injection biamperometric determination of captopril.

An automated method to determine captopril (1-[(2S)-3-mercapto-2-methylpropionyl]-L-proline) is proposed. A flow injection manifold based on the indirect biamperometric detection of the captopril by using Fe(III)/Fe(II) as an indicating redox system and a Z-shaped flow-cell configuration, was developed. The calibration curve is linear over the range 0.03-3.6 microg ml(-1) of captopril. The relative standard deviation for the determination of 0.76 microg ml(-1) of captopril is 0.97% (n = 12) and the sample throughput is 69 h(-1). This method was applied to the determination of captopril to commercially available pharmaceutical preparations.

Captopril↗
PubMed2002

Flow injection potentiometric determination of amantadine HCl.

New amantadine (Am) ion selective plastic membrane electrodes of both conventional and coated graphite types based on the ion-pair of amantadinium tetraphenylborate (Am-TPB) ion-pair are prepared. The conventional type electrode was fully characterized in terms of membrane composition, life span, pH, ionic strength and temperature. It was applied to potentiometric determination of amantadine in pure state and pharmaceutical preparation under batch and flow injection conditions. The selectivity of the electrode toward a large number of inorganic cations, sugars and amino acids was tested. The solubility product of the ion-pair and the formation constant of the precipitation reaction leading to the ion-pair formation were determined conductimetrically.

Amantadine↗
PubMed2003

Assessment of trace aluminium content in parenteral solutions by combined cloud point preconcentration-flow injection inductively coupled plasma optical emission spectrometry.

A micelle-mediated phase separation without added chelating agents to preconcentrate trace levels of aluminium in parenteral solutions as a prior step to its determination by flow injection inductively coupled plasma optical emission spectrometry has been developed. The enrichment step is based on the cloud point extraction of aluminium with the non-ionic surfactant polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5). The chemical variables affecting the sensitivity of the extractive-spectrometric procedure were studied in detail. After optimization, a preconcentration factor of 200 and a %E higher than 99.9 were achieved. The detection limit (DL) value of aluminium for the preconcentration of 50 ml of parenteral solution was 0.25 microgl(-1). The calibration graph using the preconcentration system for aluminium was linear with a correlation coefficient of 0.9997 at levels near the DLs up to at least 200 microgl(-1). The developed hyphenated assay, which thoroughly satisfies the typical requirements for pharmaceutical control processes, is appropriate to monitor the aluminium concentration in parenteral nutrition.

Aluminum↗