Flow injection amperometric determination of procaine in pharmaceutical formulation using a screen-printed carbon electrode

A rapid and simple method for procaine determination was developed by flow injection analysis (FIA) using a screen-printed carbon electrode (SPCE) as amperometric detector. The present method is based on the amine/hydroxylamine oxidation from procaine monitored at 0.80 V on SPCE in sodium acetate solution pH 6.0. Using the best experimental conditions assigned as: pH 6.0, flow rate of 3.8 mL min(-1), sample volume of 100 mu L and analytical path of 30 cm it is possible to construct a linear calibration curve from 9.0 x 10(-6) to 1.0 x 10(-4) mol L-1. The relative standard deviation for 5.0 x 10(-5) mol L-1 procaine (15 repetitions using the same electrode) is 3.2% and detection limit calculated is 6.0 x 10(-6) mol L-1. Recoveries obtained for procaine gave a mean values from 94.8 to 102.3% and an analytical frequency of 36 injections per hour was achieved. The method was successfully applied for the determination of procaine in pharmaceutical formulation without any pre-treatment, which are in good accordance with the declared values of manufacturer and an official method based on spectrophotometric analysis. (c) 2006 Elsevier B.V. All rights reserved.

A new approach for determining stability constants of metal ion complexes in aquatic systems based on flow injection-ion exchange-flame atomic absorption spectrometry coupling

A method based an ion exchange(IE)-atomic absorption spectrometry(AAS) coupled by flow techniques, allowing the determination of formation constants of, at least, the first species of complex systems, in aqueous solution, was developed.The IE-AAS coupling reduces significantly the number of experimental steps in comparison with IE batch methods, resulting in an important increase in analytical rate. The method is simple both from experimental and computational points of view, making possible its utilization by workers without special expertise in the field of complex equilibria in solution. on the other hand, taking into account mainly the amount of hollow cathode lamps available to date, the developed procedure may be applied, within certain limitations, to the study of many systems whose features prevent the use of traditional approaches.

High current-density anodic electro-dissolution in flow-injection systems for the determination of aluminium, copper and zinc in non-ferroalloys by flame atomic absorption spectrometry

An automatic Procedure with a high current-density anodic electrodissolution unit (HDAE) is proposed for the determination of aluminium, copper and zinc in non-ferroalloys by flame atonic absorption spectrometry, based on the direct solid analysis. It consists of solenoid valve-based commutation in a flow-injection system for on-line sample electro-dissolution and calibration with one multi-element standard, an electrolytic cell equipped with two electrodes (a silver needle acts as cathode, and sample as anode), and an intelligent unit. The latter is assembled in a PC-compatible microcomputer for instrument control, and far data acquisition and processing. General management of the process is achieved by use of software written in Pascal. Electrolyte compositions, flow rates, commutation times, applied current and electrolysis time mere investigated. A 0.5 mol l(-1) HNO3 solution was elected as electrolyte and 300 A/cm(2) as the continuous current pulse. The performance of the proposed system was evaluated by analysing aluminium in Al-allay samples, and copper/zinc in brass and bronze samples, respectively. The system handles about 50 samples per hour. Results are precise (R.S.D < 2%) and in agreement with those obtained by ICP-AES and spectrophotometry at a 95% confidence level.

Direct and simultaneous determination of As, Cu, and Pb in Brazilian sugar cane spirits by graphite furnace AAS using Tungsten permanent modifier with Co-injection of Pd/Mg(NO3)(2)

A method was developed using the multi-element graphite furnace atomic absorption spectrometry technique for the direct and simultaneous determination of As, Cu, and Pb in Brazilian sugar cane spirit (cachaqa) samples. Also employed was the end-capped transversely heated graphite atomizer (THGA) with platforms pre-treated with W permanent modifier and co-injection of Pd/Mg(NO3)(2). Pyrolysis and atomization temperature curves were established in a cachaqa medium (1+1; v/v) containing 0.2% (v/v) HNO3 and spiked with 20 mu g L-1 As and Pb and 200 mu g L-1 Cu. The effect of the concentration of major elements usually present in cachaqa matrices (Ca, Mg, Na, and K) and ethanol on the absorbance of As, Cu, and Pb was investigated. Analytical working solutions of As, Cu, and Pb were prepared in 10% (v/v) ethanol plus 5.0 mg L-1 Ca, Mg, Na, and K. Acidified to 0.2% (v/v) HNO3, these solutions were suitable to build calibration curves by matrix matching. The proposed method was applied to the simultaneous determination of As, Cu, and Pb in commercial sugar cane spirits. The characteristic mass for the simultaneous determination was 16 pg As, 119 pg Cu, and 28 pg Pb. The pretreated tube lifetime was about 450 firings. The limit of detection (LOD) was 0.6 mu g L-1 As, 9.2 mu g L-1 Cu, and 0.3 pig L-1 Pb. The found concentrations varied from 0.81 to 4.28 mu g L-1 As, 0.28 to 3.82 mg L-1 Cu and 0.82 to 518 mu g L-1 Pb. The recoveries of the spiked samples varied from 94-112% (As), 97-111% (Cu), and 95-101% (Pb). The relative standard deviation (n=12) was 6.9%, 7.4%, and 7.7% for As, Cu, and Pb, respectively, present in a sample at 0.87 mu g L-1, 0.81 mg L-1, and 38.9 mu g L-1 concentrations.

Anti-inflammatory efficacy of a single posterior subtenon injection of triamcinolone acetonide versus prednisolone acetate 1% eyedrops after pars plana vitrectomy

Purpose: To compare the safety and anti-inflammatory efficacy of a single posterior subtenon injection of triamcinolone acetonide (TA) with prednisolone acetate 1% eyedrops after pars plana vitrectomy (PPV).Methods: the study included 40 consecutive phakic eyes of 40 patients undergoing PPV for non-clearing vitreous haemorrhage with attached retina (verified by echography), epiretinal membrane or macular hole. At the end of the surgical procedure, eyes were randomized to receive either a single posterior subtenon injection of TA (40 mg in 1 ml) plus sham eyedrops (prednisolone acetate 1% vehicle) postoperatively (group TA), or a posterior subtenon sham injection (1 ml balanced salt solution) plus prednisolone acetate 1% eyedrops postoperatively (group ED).Results: There was no difference in the severity of anterior chamber cell and flare between the two groups at any time-point during the study period (p > 0.05). Separate within-group analysis revealed a significant decrease in anterior chamber cell and flare from postoperative day 1 to postoperative days 7, 14 and 28 in both groups (p < 0.05). There was no difference in pain, photophobia, conjunctival erythema, ciliary flush or chemosis scores between the two groups at any time-point during the study period (p > 0.05). Steroid-induced intraocular hypertension was not observed in either group.Conclusions: A single posterior subtenon injection of TA can be as effective and safe as a 4-week regimen of prednisolone acetate 1% eyedrops in controlling intraocular inflammation after PPV.

CHARACTERISTICS OF ARTERIAL-HYPERTENSION IN RESPONSE TO BOLUS INJECTION OF PHENYLEPHRINE IN ATROPINIZED PATIENTS

The changes of arterial pressure promoted by bolus injection of 50 mg phenylephrine (PHE) were studied in 20 atropinized patients (5 normal subjects, 13 patients with mitral valve disease, 1 patient with essential arterial hypertension and 1 patient with hypertrophic cardiomyopathy) submitted to routine catheterism. Patients with aortic valve disease, left ventricular outflow tract obstruction and intracardiac shunt were excluded from the study. All patients were in sinus rhythm, without heart failure. Arterial pressure started to increase at 14.8 +/- 5.4 s (range, 5.6 to 27 s; mean +/- SD) after PHE. There was an increase of 37.8 +/- 16.7 mmHg (range, 12.5 to 70 mmHg) in systolic pressure and of 26.6 +/- 11.1 mmHg (range, 7.5 to 42.5 mmHg) in diastolic pressure. Peak hypertension was attained at 36.6 +/- 16.4 s (range, 10.8 to 64.9 s) and hypertension continued for 176 +/- 92 s (range, 11 to 365 s). Heart rate was 114 +/- 21 bpm before PHE and 111 +/- 21 bpm (P<0.05) after PHE. There were no adverse events associated with intravenous PHE injection in any patient, in accordance with the general view that bolus injection of PHE is a safe and practical maneuver to promote arterial hypertension.

Comparison of accuracy between compression- and injection-molded complete dentures

Statement of problem. A clinically significant incisal pin opening may occur after processing complete dentures if a compression molding technique is used. To recover the proper vertical dimension of occlusion, a time-consuming occlusal adjustment is necessary that often destroys the anatomy of the artificial teeth. A new injection molding process claims to produce dentures that require few, if any, occlusal adjustments in the laboratory after processing.Purpose. This laboratory study compared incisal pin opening, dimensional accuracy, and laboratory working time for dentures fabricated by this new injection system with dentures constructed by the conventional compression molding technique.Material and methods. Two groups of 6 maxillary and 6 mandibular dentures were evaluated as follows: group 1 (control), Lucitone 199, compression molded with a long cure cycle; and group 2, Lucitone 199, injection molded with a long cure. Incisal pin opening was measured with a micrometer immediately after deflasking. A computerized coordinate measuring machine was used to measure dimensional accuracy of 3-dimensional variations in selected positions of artificial teeth in 4 stages of denture fabrication. Analysis of variance (ANOVA) and t tests were performed to compare the groups.Results. A significant difference was found in pin opening between groups (t test). Horizontal dimensional changes evaluated with repeated measures ANOVA revealed no significant differences between groups. However, analysis of vertical dimensional changes disclosed significant differences between the groups. There was no appreciable difference in laboratory working time for flasking and molding denture bases between the injection and compression molding techniques when polymethyl methacrylate resin was used.Conclusion. The injection molding method produced a significantly smaller incisal pin opening over the standard compression molding technique. The injection molding technique, using polymethyl methacrylate, was a more accurate method for processing dentures. There were no appreciable differences in laboratory working time between the injection and compression molding techniques.

Sympathetic hyperactivity, respiratory failure, pruritus, and anesthesia after unintentional epidural injection of potassium chloride: Case report

Background and Objectives. A combination of epidural and general anesthesia has been widely used to attenuate the surgical stress response and to provide postoperative analgesia. This case report illustrates the use of this anesthetic technique. Analgesia was induced with local anesthetic in the immediate postoperative period using unintentional 19.1% potassium chloride (KCI) as diluent. Methods. An ASA I male patient was scheduled for surgical correction of idiopathic megaesophagus under continuous epidural anesthesia combined with general anesthesia. In the postoperative period, while preparing 10 mt 0.125% bupivacaine to be administered through the epidural catheter for pain control, 5 mt 19.1% KCI was unintentionally used as diluent, resulting in a 9.55% potassium solution concentration. Results. The patient developed warmness of the lower limbs, tachycardia, hypertension, intense pruritus on the chest, agitation, exacerbation of sensory and motor blocks, and respiratory failure secondary to pulmonary edema, requiring ventilatory support. Total recovery was observed after 24 hours. Conclusions. Epidurally injected potassium leads to severe clinical manifestations caused by autonomic dysfunction, spinal cord irritation, and possible release of histamine. Despite continuous recommendations, ampule misidentification still happens in hospitals, frequently leading to serious accidents.

Density-dependent coupling constants and charge symmetry breaking

The effect of the medium in the coupling constants implicate in a charge symmetry breaking on nuclear interactions. The amount of energy due to this modification can explain the Nolen-Schiffer anomaly.

Evidence of room temperature charge-density wave behavior and glass-like states in pressed pellets of lightly doped poly (3-methyl thiophene)

We show room temperature charge-density wave (CDW) characteristics in d.c. and a.c. electric data in pressed pellets of lightly doped poly(3-methylthiophene). The possibility of a Peierls glass is discussed and metastables states are observed. D.C. and A.C. data also show a state with negative differencial resistance.

A flow-injection-ICP system sequential multielemental analysis with simultaneously mercury(II) preconcentration step

A flow-injection system for multielemental analysis with a mercury(II) preconcentration step using a resin Chelite-S(R)(Serva Feinbiochemica Heidelberg, Part No. 41709) packed minicolumn by inductively coupled plasma atomic emission spectroscopy is described. A mercury reductive elution procedure with a mixture of SnCl2/HCl was used, which allows use of 6 mol/L HCl solution instead of concentrated hydrochoric acid. The main parameters related to ICP operation, such as radio frequency power (950-1750 W), auxiliary argon flow (0.0-1.5 L/min) and spray chamber nebulizer pressure (15-35 psi), were studied. Optimization of the FIA system was reached by defining the best eluent carrier stream (1.4-2.8 mL/min), Hgdegrees carrier stream (10-40 mL min(-1)), loading time (0.5-4.0 min), sample flow rate (1.25-10.0 mL/min), temperature of reactor gas liquid separator (GLS) (25-75 degreesC) and eluent volume (50-350 muL). Throughput is around 30 samples per hour for analytical solutions within the range 50-2500 ng Hg(II)/L. Results from certified material showed good precision (RSD < 3%, n = 12) and no statistical difference was observed for real samples analyzed by AAS and by the proposed system.

Evaluation of Bi as internal standard to minimize matrix effects on the direct determination of Pb in vinegar by graphite furnace atomic absorption spectrometry using Ru permanent modifier with co-injection of Pd/Mg(NO3)(2)

Bismuth was evaluated as an internal standard for the direct determination of Pb in vinegar by graphite furnace atomic absorption spectrometry using Ru as a permanent modifier with co-injection of Pd/Mg(NO3)(2). The correlation coefficient of the graph plotted from the non-nalized absorbance signals of Bi versus Pb was r=0.989. Matrix effects were evaluated by analyzing the slope ratios between the analytical curve, and analytical curves obtained from Pb additions in red and white wine vinegar obtained from reference solutions prepared in 0.2% (v/v) HNO3, samples. The calculated ratios were around 1.04 and 1.02 for analytical curves established applying an internal standard and 1.3 and 1.5 for analvtical curves without. Analytical curves in the 2.5-15 pg L-1 Pb concentration interval were established using the ratio Pb absorbance to Bi absorbance versus analvte concentration, and typical linear correlations of r=0.999 were obtained. The proposed method was applied for direct determination of Pb in 18 commercial vinegar samples and the Pb concentration varied from 2.6 to 31 pg L-1. Results were in agreement at a 95% confidence level (paired t-test) with those obtained for digested samples. Recoveries of Pb added to vinegars varied from 96 to 108% with and from 72 to 86% without an internal standard. Two water standard reference materials diluted in vinegar sample were also analyzed and results were in agreement with certified values at a 95% confidence level. The characteristic mass was 40 pg Pb and the useful lifetime of the tube was around 1600 firings. The limit of detection was 0.3 mu g L-1 and the relative standard deviation was <= 3.8% and <= 8.3% (n = 12) for a sample containing, 10 mu L-1 Pb with and without internal standard, respectively. (C) 2007 Elsevier B.V. All rights reserved.

Evaluation of a highly sensitive amperometric biosensor with low cholinesterase charge immobilized on a chemically modified carbon paste electrode for trace determination of carbamates in fruit, vegetable and water samples

A highly sensitive amperometric biosensor for determination of carbamate pesticides directly in water, fruit and vegetable samples has been evaluated, electrochemically characterized and optimized. The biosensor strip was fabricated in screen printed technique on a ceramic support using silver-based paste for reference electrode, and platinum-based paste for working and auxiliary electrodes. The working electrode was modified by a layer of carbon paste mixed with cobalt(II) phthalocyanine and acetylcellulose. Cholinesterase (ChE) enzymes with low enzymatic charge were immobilized on this layer. The operational simplicity of the biosensor consists in that a small drop (similar to 50 mu l) of substrate or sample is deposited on a horizontally positioned biosensor strip representing the microelectrochemical cell. The working potential of the biosensor was 370 mV versus Ag/AgI on a ship reference electrode preventing the interference of electroactive species which are oxidable at more positive potentials. The biosensor was applied to investigate the degradation of two reference ChE inhibitors in freeze dried water under different storage conditions and for direct determination of some N-methylcarbamates (NMCs) in fruit and vegetable samples at ppb concentration levels without any sample pretreatment. A comparison of the obtained results for the total carbamate concentration was done against those obtained using HPLC measurements. (C) 1999 Elsevier B.V. B.V. All rights reserved.