Willian Toito Suarez

Flow-Injection spectrophotometric system for captopril determination in pharmaceuticals

A simple, accurate and precise flow-injection spectrophotometric procedure is reported for the determination of captopril in pharmaceutical formulations. In this procedure, captopril was oxidized by iron(III) and the iron(II) produced was spectrophotometrically monitored as iron(II)-1,10-phenantroline complex at 540 nm. The analytical curve for captopril was linear in the concentration range from 1.0 × 10-5 to 8.0 × 10-4 mol L-1 with a detection limit of 5.0 × 10-6 mol L-1. The recovery of this analyte in five samples ranged from 98.5 to 102.4%. The analytical frequency was sixty determinations per hour and the RSD was less than 0.2% for a captopril concentration of 4.0 × 10-4 mol L-1 (n = 10). A paired t-test showed that all results obtained for captopril in commercial formulations using the proposed flow injection procedure and a potentiometric procedure agreed at the 95% confidence level.

Flow injection turbidimetric determination of acetylcysteine in pharmaceutical formulations using silver nitrate as precipitant reagent

A simple, accurate and precise flow-injection turbidimetric procedure is reported for the determination of acetylcysteine in pharmaceutical formulations. The procedure is based on the precipitation of acetylcysteine with silver nitrate solution in acid medium and the insoluble salt produced was monitored at 410 nm. The analytical curve for acetylcysteine was linear in the concentration range from 1.0 × 10-4 to 1.0 × 10-3 mol L-1 with a detection limit of 5.0 × 10-5 mol L-1. The sampling rate was 60 h-1 and the relative standard deviations (RSDs) were less than 2.0% for 1.0 × 10-4 and 5.0 × 10-4 mol L-1 acetylcysteine solutions (n=10). The recovery of this analyte in four samples ranged from 97.6 to 103 %. A paired t-test showed that all results obtained for acetylcysteine in pharmaceutical products using the proposed flow-injection procedure and the official procedure agreed at the 95% confidence level.

Flow-Injection Spectrophotometric Determination of N-acetylcysteine in Pharmaceutical Formulations with On-Line Solid-Phase Reactor Containing Zn(II) Phosphate Immobilized in a Polyester Resin

Abstract A flow‐injection spectrophotometric procedure was developed for determining N‐acetylcysteine in pharmaceutical formulations. The sample was dissolved in deionized water and 400 µl of the solution was injected into a carrier stream of 1.0×10−2 mol l−1 sodium borate solution. The sample flowed through a column (70 mm length×2.0 mm i.d.) packed with Zn3(PO4)2 immobilized in a polymeric matrix of polyester resin and Zn(II) ions were released from the solid‐phase reactor because of the formation of the Zn(II) (N‐acetylcysteine)2 complex. The mixture merged with a stream of borate buffer solution (pH 9.0) containing 5.0×10−4 mol l−1 Alizarin red S and the Zn(II)Alizarin red complex formed was measured spectrophotometrically at 540 nm. The analytical curve was linear in the N‐acetylcysteine concentration range from 3.0×10−5 to 1.5×10−4 mol l−1 (4.9 to 24.5 µg ml−1) with a detections limit of 8.0×10−6 mol l−1 (1.3 µg ml−1). The relative standard deviations (RSDs) were smaller than 0.5% (n=10) for solutions containing 5.0×10−5 mol l−1 (8.0 µg ml−1) and 8.0×10−5 mol l−1 (13.0 µg ml−1) of N‐acetylcysteine, and the analytical frequency was 60 determinations per hour. A paired t‐test showed that all results obtained for N‐acetylcysteine in commercial formulations using the proposed flow‐injection procedure and a comparative procedure agreed at the 95% confidence level.

Conductometric Determination of N-acetylcysteine in Pharmaceutical Formulations Using Copper(II) Sulphate as Titrant

Abstract A simple, precise, rapid, and low-cost conductometric method for N-acetylcysteine determination in pharmaceutical formulations is proposed. N-acetylcysteine present in pharmaceuticals containing known quantities of the drug was conductometrically titrated in aqueous solution with copper(II) sulphate using a conductometric cell coupled to an autotitrator. No interferences were observed in the presence of common components of the tablets such as sodium monophosphate, saccharine, sodium benzoate, sucrose, and fructose. Recoveries of N-acetylcysteine from various tablet dosage formulations ranging from 98.3 to 102.0% were obtained.

Flow Injection Spectrophotometric Determination of N-Acetylcysteine and Captopril Employing Prussian Blue Generation Reaction

A novel flow injection procedure to determine N-acetylcysteine and captopril in pharmaceutical formulations is proposed. The flow procedure developed was based on oxidation of the analytes by Fe(III) in acidic medium and subsequent reaction of the Fe(II) generated with excess hexacyanoferrate(III) to produce soluble Prussian blue (KFe[Fe(CN)6]) measured at 700 nm. Detection limits of 1.0 × 10−5 mol L−1 and 3.0 × 10−5 mol L−1 for N-acetylcysteine and captopril, respectively, were found. The sample throughput was 70 h−1 for both analytes and the results obtained were in agreement at a 95% confidence level with those obtained using reference methods.

A compact miniaturized continuous flow system for the determination of urea content in milk

AbstractA multicommutation-based flow system with photometric detection was developed, employing an analytical microsystem constructed with low temperature co-fired ceramics (LTCC) technology, a solid-phase reactor containing particles of Canavalia ensiformis DC (urease source) immobilized with glutaraldehyde, and a mini-photometer coupled directly to the microsystem which monolithically integrates a continuous flow cell. The determination of urea in milk was based on the hydrolysis of urea in the solid-phase reactor and the ammonium ions produced were monitored using the Berthelot reaction. The analytical curve was linear in the urea concentration range from 1.0u2009×u200910−4 to 5.0u2009×u200910−3xa0molxa0L−1 with a limit of detection of 8.0u2009×u200910−6xa0molxa0L−1. The relative standard deviation (RSD) for a 2.0u2009×u200910−3xa0molxa0L−1 urea solution was lower than 0.4% (nu2009=u200910) and the sample throughput was 13xa0h−1. To check the reproducibility of the flow system, calibration curves were obtained with freshly prepared solutions on different days and the RSD obtained was 4.7% (nu2009=u20096). Accuracy was assessed by comparing the results of the proposed method with those from the official procedure and the data are in close agreement, at a 95% confidence level.n

A compact miniaturized flow system based on low-temperature co-fired ceramic technology coupled to LED mini-photometer for determination of dipyrone in pharmaceutical formulations

In this work, an analytical microsystem based on LTCC (low-temperature co-fired ceramic) technology with monolithic incorporation of an optical flow cell for determination of dipyrone in pharmaceuticals is described. The detection system is based on the formation of a blue chromophore between dipyrone and Fe(III) photometrically monitored at 630 nm using a lab-made LED mini-photometer constructed with a light emitting diode as a radiation source and a Si photodiode as a detector. The lab-made mini-photometer elaborated presented a good performance in regard to high signal/noise ratio, low drift and good sensitivity. The analytical curve was linear in the dipyrone concentration range from 1.0 × 10 -4

Flow-injection spectrophotometric determination of captopril in pharmaceutical formulations using a new solid-phase reactor containing AgSCN immobilized in a polyurethane resin

A simple flow-injection analysis procedure was developed for determining captopril in pharmaceutical formulations employing a novel solid-phase reactor containing silver thiocyanate immobilized in a castor oil derivative polyurethane resin. The method was based on silver mercaptide formation between the captopril and Ag(I) in the solid-phase reactor. During such a reaction, the SCN- anion was released and reacted with Fe3+, which generated the FeSCN2+ complex that was continuously monitored at 480 nm. The analytical curve was linear in the captopril concentration range from 3.0 × 10-4 mol L-1 to 1.1 × 10-3 mol L-1 with a detection limit of 8.0 × 10-5 mol L-1. Recoveries between 97.5% and 103% and a relative standard deviation of 2% for a solution containing 6.0 × 10-4 mol L-1 captopril (n = 12) were obtained. The sample throughput was 40 h-1 and the results obtained for captopril in pharmaceutical formulations using this procedure and those obtained using a pharmacopoeia procedure were in agreement at a 95% confidence level.

Determinação condutométrica de cloridrato de metformina em formulações farmacêuticas empregando nitrato de prata como titulante

A simple, precise, rapid and low-cost conductometric titration method for the determination of metformin hydrochloride (MET) in pharmaceuticals using silver nitrate as titrant is proposed. The method was based on the chemical reaction between the chloride of metformin hydrochloride molecule and Ag(I) ions, yielding the precipitate AgCl(s). The method was applied for MET determination in three pharmaceuticals and the obtained results with proposed method were in close agreement with those results obtained using an official method of the British Pharmacopoeia, at a 95% confidence level.

Flow Injection Spectrophotometric Determination of Dipyrone in Pharmaceutical Formulations Using Fe(III) as Reagent

A flow injection spectrophotometric procedure with symmetric merging zones for dipyrone determination in pharmaceutical formulations is proposed. The determination is based on the formation of a blue complex (monitored at a wavelength of 642 nm) yield in the complexation reaction of dipyrone with Fe(III) in acid medium. Under optimum conditions, a calibration curve was obtained from 3.5 to 281 mg L−1 with a detection limit of 2.8 mg L−1 and the samples throughput was 80 h−1. The analytical results obtained for commercial formulation samples by applying the proposed method were in good agreement with labeled values and those obtained by a comparative procedure at a 95% confidence level.