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A N Araújo

Publications and source records attributed to A N Araújo.

7 recordsLinked to original sources

Photo-induced chemiluminometric determination of Karbutilate in a continuous-flow multicommutation assembly.

The present paper deals with the chemiluminescent determination of the herbicide Karbutilate on the basis of its previous photodegradation by using a low-pressure Hg lamp as UV source in a continuous-flow multicommutation assembly (a solenoid valves set). The pesticide solution was segmented by a solenoid valve and sequentially alternated with segments of the 0.001 mol l(-1) of NaOH solution, the suitable media for the formation of photo-fragments; then it passes through the photo-reactor and was lead to the flow-cell after being divided in small segments which were sequentially alternated with the oxidizing system; 2 x 10(-5) mol l(-1) of potassium permanganate in 0.2% pyrophosphoric acid. The studied calibration range, from 0.1 microg l(-1) to 65 mg l(-1), resulted in a linear behaviour over the range 20 microg l(-1)-20 mg l(-1) and fitting the linear equation: I=(1180+/-30)C+(15+/-5) with the correlation coefficient 0.9998. The limit of detection was 10 microg l(-1) and the sample throughput 17 h(-1). After testing the influence of a large series of potential interfering species, the method was applied to water and human urine samples.

Calibration↗

Application of sequential injection analysis to pharmaceutical analysis.

Sequential injection analysis is a well established tool for automation of pharmaceutical analysis. A short historical background of this technique is given as well as a brief discussion on the basic principles and potentials. The current applications of SIA in the pharmaceutical analysis are also described and discussed. The manifolds developed offer good analytical characteristics and are suitable for analysis of drug formulations, process analysis, drug-dissolution, drug-release testing and functional assays for screening potential drugs. The results obtained are in good agreement with those furnished by the application of the reference methods presented in the pharmacopoeias.

Biological Availability↗

Clavulanate-selective electrodes--application to pharmaceutical formulations.

The construction and assessment of a clavulanate anion-selective electrode and its application to the analysis of pharmaceutical formulations by direct potentiometry are described. The electrode, prepared without inner reference solution, was fabricated by use of a PVC membrane, with bis(triphenyl-phosphoranylidene)ammonium clavulanate as ion-exchanger dissolved in 2-nitrophenyl octyl ether as intermediate solvent and p-t-octylphenol as additive. The response of the electrode was linearly dependent on concentration within the range 2.4 x 10(-3)-1 x 10(-1) mol dm(-3) (ionic strength adjusted to 0.1 mol dm(-3)); the slope of the calibration plot was -59.4+/-0.9 mV decade(-1) and the reproducibility +/-0.6 mV day(-1). The response time was less than 20 s. Relative errors were <3.5% when results from analysis by direct potentiometry were compared with those from the reference method.

Anti-Bacterial Agents↗

Potentiometric determination of acetylsalicylic acid by sequential injection analysis (SIA) using a tubular salicylate-selective electrode.

This paper deals with the development of an automated procedure for formulation assays and dissolution tests based on a sequential injection analysis (SIA) system involving an ion-selective electrode as sensing device. Construction of a tubular salicylate (Sal) selective electrode suitable for potentiometric determination of acetylsalicylic acid (Asa) in pharmaceutical formulations is described. The flow-through electrode is formed by a PVC membrane containing 29.2% (w/w) PVC, 5.8% (w/w) tetraoctylammonium salicylate (ionic sensor), 58.5% o-nitrophenyloctylether (plasticizer) and 6.5% (w/w) p-tert-octylphenol (stabilising additive which increases electrode selectivity). The calibration range is 0.05--10 mM Sal, the limit of detection (LOD) is 0.05 mM Sal, the slope is 56.0 mV per decade at 22 degrees C. The R.S.D. is 0.20% (15 readings) when determining 2.5 mM Sal in standard solution. The electrode is used for sensing Asa after its on-line chemical hydrolysis to Sal in a SIA system. The sampling rate is 6 h(-1) but for the dissolution tests the frequency is increased to 20 h(-1). The SIA set-up is employed for the assay of Asa in plain tablets, composed tablets and effervescent tablets and for performing dissolution tests of normal and sustained release tablets. Results obtained by this technique compare well with those required by the US Pharmacopoeia XXIV.

Aspirin↗

Multi-task flow system for potentiometric analysis: its application to the determination of vitamin B6 in pharmaceuticals.

A flow set-up based on the sequential injection analysis concept was designed, aiming at increased automation and robustness of procedures related with potentiometric detection in pharmaceutical control. In this sense, programmable set-up calibration, ion-selective electrode characterization, standard addition techniques and titration procedures could be carried out without any stock solutions conventional handling or modification on the physical structure of the flow system. Evaluation of a flow-through vitamin B6 selective electrode and its application to routine analysis of pharmaceuticals were selected as models to demonstrate the system potentialities. The system ability to generate in-line calibrating solutions was verified by comparing the results with those obtained with solutions prepared by the manual procedure. The vitamin B6 determination in pharmaceutical products was carried out and in-line performed recoveries gave values within 97.4-103.5%. The system ability to perform titrations was ascertained using the precipitation reaction of vitamin B6 with tetraphenylborate. Other profitable features such as lower reagent consumption with a low effluent generation volume were also achieved.

Calibration↗

Flow injection analysis of inorganic cationic species in serum and urine.

This paper describes three flow injection analysis (FIA) systems for the automatic determination of sodium, potassium, lithium, calcium, magnesium, zinc, copper and iron in certain biological fluids and compares the results obtained to those of flame photometry and atomic absorption spectrometry. The set-ups were designed to allow the samples to be prepared in the same manner as that used for batch procedures with the same analytical instrument. For determinations requiring a high sample dilution, it was found of definite advantage to split the stream and pass large amounts of liquid through the detection systems. The comparison of the results obtained by FIA and conventional methods yielded correlation coefficients in the range 0.990 to 0.999. The proposed methodology show good precision, with variation coefficients between 0.5% to 5%.

Calcium↗

Monosegmented flow-analysis of serum cholesterol.

A monosegmented flow system is designed for enzymatic spectrophotometric determination of cholesterol in blood serum. The sample (4.5 microliters), enzymatic reagent (150 microliters) and an air plug (100 microliters) are simultaneously inserted into a carrier stream buffered to pH 7.4 (potassium dihydrogenphosphate). In order to avoid the step of air removal, a relocating detector was used. This system handles about 42 samples per hour, yielding precise results (R.S.D. usually < 3.0%). Sensitivity is 46 mAU 1/mmol (mAU stands for milliabsorbance units), being the method linear up to 10.3 mmol/l cholesterol. Accuracy was assessed by running 30 samples already analysed by a conventional procedure: no statistical difference between methods was found at the 95% confidence level.

Buffers↗