Biomedical subjects

M G Sales

Publications and source records attributed to M G Sales.

11 recordsLinked to original sources

PubMed2001

Determination of tartaric acid in wines by FIA with tubular tartrate-selective electrodes.

A flow injection analysis (FIA) system comprising a tartrate-(TAT) selective electrode has been developed for determination of tartaric acid in wines. Several electrodes constructed for this purpose had a PVC membrane with a complex of quaternary ammonium and TAT as anion exchanger, a phenol derivative as additive, and a more or less polar mediator solvent. Characterization of the electrodes showed behavior was best for membranes with o-nitrophenyl octyl ether as solvent. On injection of 500 microL into a phosphate buffer carrier (pH = 3.1; ionic strength 10(-2) mol/L) flowing at 3 mL/min, the slope was 58.06 +/- 0.6 with a lower limit of linear range of 5.0 x 10(-4) mol/L TAT and R2 = 0.9989. The interference of several species, e.g. chloride, bromide, iodide, nitrate, gallic acid, tannin, sucrose, glucose, fructose, acetate, and citrate, was evaluated in terms of potentiometric selectivity coefficients. The Hofmeister series was followed for inorganic species and the most interfering organic ion was citrate. When red and white wines were analyzed and the results compared with those from an independent method they were found to be accurate, with relative standard deviations below 5.0%.

Electrodes↗

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↗

PubMed2001

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↗

PubMed2001

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↗

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

Differential expression of laminin isoform (alpha2), integrins (alpha3beta1 and alpha6beta4) and cytokeratin 20 in H. pylori gastritis.

The expression of laminin-1 chains (beta1 and gamma1), laminin-2 (merosin), integrin receptors to laminin (alpha3beta1 and alpha6beta4) and cytokeratin (CK20) were studied by immunohistochemical methods in gastric biopsies from antrum of 25 patients. H. pylori gastritis was found in 19 cases and intestinal metaplasia (IM) in four from these 19. Another 13 biopsies, all with IM were immunostained to laminin-2. Laminin-1 chains in normal and gastritis areas without IM were expressed as a strong, linear and continuous deposit in the basement membranes of the superficial and glandular epithelium. In metaplastic glands the reactivity to laminin-1 chains was decreased. Merosin was discontinuous when a moderate to accentuated H. pylori glandular colonization was present. Samples with IM were negative to laminin-2. The alpha3beta1 and alpha6beta4 integrins were negative only in IM gastric biopsies. The CK20 immunoreactivity was strong and homogeneous in the cells at the tip and the upper portion of foveolae in normal areas and in gastritis with IM the reactivity to CK 20 was heterogeneous. A differential expression of laminin isoforms is related to inflammation and subsequent IM caused by H. pylori. The alterations of alpha3beta1 and alpha6beta4 parallel both modifications in merosin and CK20 expression in H. pylori chronic gastritis.

Adult↗

PubMed2000

Flow-injection analysis of dopamine in injections with a periodate-selective electrode.

Dopamine determination in pharmaceutical preparations based on its oxidation with periodate (IO(4)(-)) using a new IO(4)(-)-selective electrode under flow conditions is presented. An electrode with a tubular configuration, no internal reference solution, and a PVC (31. 2%) membrane, with metaperiodate bis(triphenylphosphoranylidene)ammonium (1.3%) as ion exchanger and 2-nitrophenyloctylether (67.5%) as mediator solvent, was used. Optimization procedures were directed at potentials versus dopamine readings instead of potential versus the remaining IO(4)(-). This approach was achieved by selecting a 50-cm reactor and an overall flow of 7 mL/min, and injecting 70 microL of dopamine standards in a 3.0 x 10(-4) M IO(4)(-) solution. Under these conditions, a linearity range of 8.0 x 10(-3) to 2.7 x 10(-1) g/L, with a slope of 310.1 +/- 7.4 mV L g(-1) and a reproducibility of +/-0.4 mV, were recorded (n = 8). Interference from common excipients was negligible. Under these conditions, analysis of dopamine injections (n = 12) presenting 200 mg/injection gave average and standard deviation values of 201.0 and 3.3 mg/injection, respectively. A simple and inexpensive flow-injection analysis (FIA) manifold, with a good potentiometric detector, enabled the analysis of 200 samples/h without requiring pretreatment procedures. Comparison with the dopamine injection analysis in the United States Pharmacopoeia monograph showed good accuracy, with a relative deviation of -0.2%.

Dopamine↗

PubMed1998

Cefuroxime selective electrodes for batch and FIA determinations in pharmaceutical preparations.

Different cefuroxime selective electrodes, without internal reference solution and comprising PVC membranes, were constructed and evaluated. Membranes were prepared with cefuroxime tetraoctylammonium (A) or cefuroxime bis(triphenylphosphoranylidene)ammonium (B) as ion-exchanger, 2-nitrophenyl octyl ether (X) or bis(2-ethylhexyl)sebacate (Y) as plasticizing mediator solvent and 4-tert-otcylphenol (TOP) as additive. From the comparative evaluation of the described electrodes, membranes comprising 2-nitrophenyl octyl ether, cefuroxime tetraoctylammonium and 4-tert-otcylphenol presented better working characteristics. For these electrodes (type XA-TOP), with a lifetime > 5 months, a lower limit of linear range of 2.8 x 10(-4) M, a practical detection limit of 1.3 x 10(-4) M, a reproducibility of approximately +/-0.6 mV day(-1) and a slope of -50.4 mV decade(-1), under H3PO4/NaH2PO4 solutions (pH 3.5; I =0.1 M), were found. The presence of the additive on the membranes was of crucial importance for the electrodes good characteristics. Interference from sulphate, chloride, nitrate, iodide, cefaclor, cefadroxil, cefazolin and cephradine, on the electrodes behaviour was evaluated. Only a slight interference from nitrate and iodide was recorded, being type XA-TOP electrodes the most selective units. Electrodes with a tubular configuration prepared with type XA-TOP membranes, aiming flow injection analysis, were also constructed. When these tubular potentiometric detectors were evaluated in a double-channel flow injection manifold, with 3.5 pH and 0.1 M ionic strength conditions, significantly better working characteristics than those of the corresponding conventional electrodes, namely higher slopes (-54.6 mV decade(-1)) and better reproducibilities (+/-0.2 mV day(-1)), were found. Both conventional and tubular type XA-TOP electrodes were used for injections analyses by batch and FIA, respectively, presenting low consumption of samples and reagents. Relative error deviations to the reference procedures <3.0% were found.

Cefuroxime↗

PubMed1997

Ion-selective electrodes for promethazine determinations in pharmaceutical preparations and application to flow injection analysis.

The construction and evaluation of PM-selective electrodes with a conventional configuration and without internal reference solution are described. Two different PVC membranes were prepared with PM tetraphenylborate dissolved in 2-nitrophenyl octyl ether (type A) or bis (2-ethylhexyl)sebacate (type B). When the electrodes were evaluated in 0.01 M ionic strength solutions, both presented linear responses from 5 x 10(-5) to 1 x 10(-2) M, slopes close to the theoretical value, practical detection limits of approximately 2 x 10(-5) M, reproducibilities of +/- 0.2 mV/day, and a quick response (< 20 s). Using phosphate buffer solutions (pH 6.0), type B electrodes presented a lower practical detection limit and a better reproducibility than type A. Selectivity against several cations was assessed by the separated solutions method, and the type B electrodes were generally more selective. The type B membrane was also used for the construction of tubular electrodes for the automatic analysis of pharmaceutical products by flow injection analysis (FIA). These tubular detectors, evaluated in a low dispersion FIA system, presented better selectivity and sensitivity than the corresponding conventional ones. Several pharmaceutical preparations were analyzed with both conventional and tubular electrodes. The results obtained by FIA presented relative deviations of < 2% when compared with those obtained from the United States Pharmacopoeia monographs.

Electrodes↗

PubMed1996

Construction and evaluation of PVC conventional and tubular tripelennamine-selective electrodes: their application in pharmaceutical preparations.

The construction and evaluation of tripelennamine conventionally-shaped ion-selective electrodes and tubular detectors for the determination of this compound in pharmaceutical formulations are described. Electrodes with conventional configuration have been constructed without an internal reference solution, using several types of immobilized ionic sensors in PVC. The different electrode membranes were prepared by using tripelennamine tetraphenylborate as ionic-exchanger, dissolved in 2-nitrophenyl octyl ether (type A), dibutylphthalate (type B) and bis-(2-ethylhexyl)sebacate (type C) as plasticizer solvents. The general working characteristics of the different types of conventional electrodes were evaluated in tripelennamine solutions, with adjusted ionic strength, showing a linear response in the concentration range of about 4 x 10(-5) - 1 x 10(-1) M and a slope near the theoretical value. The electrodes presented a fast response (> 20 s) and a high reproducibility (> or = 0.2 mV per day). The electrode selectivity in the presence of some interferents, such as sodium, potassium, lithium, ammonium, chlorpheniramine, diphenydramine, promethazine, meclizine and pentazocine, was good, particularly for those whose sensor membrane was prepared with tripelennamine tetraphenylborate dissolved in 2-nitrophenyl octyl ether (type A). Tubular detectors were also prepared using the same sensor membrane and were evaluated in a low-dispersion flow-injection manifold. Under these conditions the detectors presented response characteristics similar to those of the corresponding conventionally-shaped electrodes. The analysis of different pharmaceutical forms (creams, syrups and gels) gave good results with mean recoveries of 99.8-100.6% when the experiments were conducted by direct potentiometry and 99.9-100.4% where the same determinations were conducted by flow-injection analysis with tubular detectors.

Chemistry, Pharmaceutical↗

PubMed1995

Casein, hydrolyzed casein, and amino acids that simulate casein produce the same extent of mucosal adaptation to massive bowel resection in adult rats.

We determined the effect of the extent of protein polymerization on the intestinal hyperplastic adaptation of adult male Wistar rats after 80% resection of the jejunal-ileal segment. Rats received one of four chemically defined solid diets prepared by using casein, two casein hydrolysates of different peptide size distributions, or free amino acids simulating casein and identical in all other components for 12 d, starting 3 d after surgery. Semipaired feeding was used to ensure that the same quantity of food was ingested by each group and as a consequence, nitrogen and energy intakes were reduced to 63% of that obtained with ad libitum feeding of the casein diet to intact rats. No significant differences were demonstrable in food ingestion, weight gain, nitrogen balance, or morphometric data for the remaining jejunal and ileal segments (number of cells/villus, number of cells/crypt, and crypt cell mitosis rate). These data demonstrate that the extent of polymerization of the protein nitrogen source did not affect the hyperplastic adaptative process of the rat. Additional studies in humans are necessary to determine whether intact protein diets can be used first as a nitrogen source in nutritional support of patients with a nonspecific hyperplastic response to surgical resection before the use of expensive hydrolysates and the more expensive amino acid mixtures.

Adaptation, Physiological↗