Electrochemical, Spectrophotometric and Liquid-Chromatographic Approaches for Analysis of Tropical Disease Drugs

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Sequential injection analysis system with spectrophotometric detection for determination of norfloxacin and ciprofloxacin in pharmaceutical formulations

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Sequential spectrophotometric determination of chromium(III) and chromium(VI) using flow injection analysis

A flow injection analysis (FIA) procedure for the speciation of Cr(III) and Cr(VI) using the 1,5-diphenylcarbazide (DPC) method is presented. As Cr(III) does not interfere in the Cr(VI) - DPC reaction, both Cr(VI) and total chromium [after the on-line oxidation of Cr(III) by Ce(IV)] are sequentially determined. Cr(III) is obtained by difference. Under the experimental conditions described, the calibration graphs are linear up to 2 μg mh1 of Cr(VI) and 4 μg ml-1 of Cr(III). The detection limits found were 18 ng ml -1 for Cr(VI) and 55 ng ml-1 for Cr(III), at a signal to noise ratio of 3. The common interfering elements in the Cr(VI) - DPC reaction were investigated under dynamic FIA conditions. The FIA method was also compared with the conventional spectrophotometric procedure.

A simplified spectrophotometric method for routine analysis of saccharin in commercial noncaloric sweeteners

A simple, rapid, and sensitive spectrophotometric method for routine analysis of saccharin in commercial noncaloric sweeteners is proposed. This method is based on the reaction of saccharin with tetrachloro-p-benzoquinone (p-chloranil) accelerated by hydrogen peroxide and conducted in an ethanol:acetone (4:1) medium, producing a violet-red compound (γ max = 550 nm). Beer's law is obeyed in a concentration range of 2.05 × 10 -4 to 3.00 × 10 -3 M with an excellent correlation coefficient (r = 0.9998). The detection limit was 1.55 × 10 -5 M, and the effect of interferences on the spectrophotometric measurements was evaluated. The proposed procedure was applied successfully to the determination of saccharin in noncaloric sweeteners. Recoveries were within 99.2-104.3% with standard deviations ranging from to 0.5-1.6%. Results of the proposed method compare very favorably with those given by the high-performance liquid chromatography method recommended by the Food and Drug Administration.

A platform for designing quantitative infrared spectrophotometric method for drugs and pharmaceuticals analysis: a rediscover for an ecological and safer technique in the routine quality control laboratories

This paper describes the importance of an innovative analytical technique for drugs and pharmaceuticals quantification, using Fouriertransform infrared (FTIR) transmission spectroscopy. This method does not use organic solvents, which is one great advantage over the most common analytical methods. This fact contributes to minimize the generation of organic solvent waste by the industry and thereby reduces the impact of its activities on the environment. The method involved absorbance measurements of the band corresponding to one of the chosen group in the molecule. Obviously, the method should be validated according to ICH guidelines, showing linearity, precision, accuracy and robustness, over a concentration range, using small amounts to prepare the analyte. The validated method is able to quantify drugs and pharmaceuticals and can be used as an environmentally friendly alternative for the routine analysis in pharmaceutical industry quality control.

Thermal analysis and validation of UV and visible spectrophotometric methods for the determination of new antibiotic tigecycline in pharmaceutical product

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Flow-injection spectrophotometric determination of dipyrone in pharmaceutical formulations using ammonium molybdate as chromogenic reagent

A simple and rapid flow-injection spectrophotometric method is reported for the determination of dipyrone in pharmaceutical formulations. The method is based on the reaction of dipyrone with ammonium molybdate in acidic medium to produce blue molybdenum, which was detected spectrophotometrically at 620 nm. The analyte was determined in a single-line flow system. The calibration curve obtained was linear in the range of 5x10(-4) to 8x10(-3) mol L-1 for dipyrone concentration and the precision ( s r =1.7%) was satisfactory. The method proved to be selective and adequately sensitive. Application of the method to the analysis of pharmaceutical samples resulted in excellent accuracy; the percent mean recoveries were in the range 95.3%-101% and relative errors less than 5.0% for five pharmaceutical formulations were found.

Spectrophotometric determination of sparfloxacin in pharmaceutical formulations using bromothymol blue

A visible light spectrophotometric method is described for them determination of sparfloxacin in tablets. The procedure is based on the complexation of bromothymol blue 0.5% and sparfloxacin to form a compound of yellow colour with maximum absorption at 385 nm. The Lambert-Beer law was obeyed in the concentration range of 2-12 mg/l. The present study describes a sensitive and accurate method for the determination of the concentration of sparfloxacin in tablets. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay.

Spectrophotometric determination of ceftazidime in pharmaceutical preparations using neocuproin as a complexing agent

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Development and Validation of a UV-Spectrophotometric Method for Determination of Flucloxacillin Sodium in Capsules

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Direct and simultaneous spectrophotometric determination of Ni (II) and Co (II) using diethanoldithiocarbamate as complexing agent

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Flow-injection spectrophotometric determination of methyldopa in pharmaceutical formulations

A flow-injection spectrophotometric procedure is proposed for methyldopa determination in pharmaceutical preparations. The determination is based on formation of a yellow product (measured at 410 nm) after complexation of methyldopa with molybdate. Under optimal conditions, Beer's law is obeyed in a concentration range of 50-200 mg l(-1) methyldopa. Typical correlation between absorbance and analyte concentration was 0.9999. Usual excipients used as additives in pharmaceuticals do not interfere with the proposed method. The analytical frequency was 210 h(-1) and the relative standard deviation (R.S.D.) was <= 2% for sample solution containing 150 mg l(-1) methyldopa (n = 11). The analytical results obtained in commercial formulations by applying the proposed FIA method were in good agreement with labeled values and those obtained by the Brazilian Pharmacopoeia procedure at 95% confidence level. (C) 2005 Elsevier B.V. All rights reserved.

Spectrophotometric determination of formaldehyde with chromotropic acid in phosphoric acid medium assisted by microwave oven

In the present study. a spectrophotometric method for the determination of formaldehyde by using chromotropic acid was devised. in which the use of potentially hazardous and corrosive concentrated sulfuric acid was eliminated and advantageously C replaced by a mixture of H, concentrated H3PO4 and H2O2. The reaction between formaldehyde and chromotropic acid (CA) in a cone phosphoric acid medium was accelerate by irradiating the mixture with microwave energy for 35 s (1100 W), producing a violetred compound (lambda(max)=570 nm). Beer's Law is obeyed in a concentration range of 0.8-4.8 mg 1(-1) of formaldehyde with a good correlation coefficient (r = 0.9968). The proposed method was applied in the analysis of formaldehyde in commercial disinfectants. Recoveries were within 98.0-100.4%, with standard deviations ranging from 0.03 to 0.13%. (C) 2003 Elsevier B.V All rights reserved.

Simple and fast spectrophotometric determination of H2O2 in photo-Fenton reactions using metavanadate

This work proposes a spectrophotometric method for the determination of hydrogen peroxide during photodegradation reactions. The method is based on the reaction of H2O2 with amonium metavanadate in acidic medium, which results in the formation of a red-orange color peroxovanadium cation, with maximum absorbance at 450 nm. The method was optimized using the multivariate analysis providing the minimum concentration of vanadate (6.2 mmol L-1) for the maximum absorbance signal. Under these conditions, the detection limit is 143 mu mol L-1. The reaction product showed to be very stable for samples of peroxide concentrations up to 3 mmol L-1 at room temperature during 180 h. For higher concentrations however, samples must be kept refrigerated (4 degrees C) or diluted. The method showed no interference of Cl- (0.2-1.3 mmol L-1), NO3- (0.3-1.0 mmol L-1), Fe3+, (0.2-1.2 mmol L-1) and 2,4-dichlorophenol (DCP) (0.2-1.0 mmol L-1). When compared to iodometric titration, the vanadate method showed a good agreament. The method was applied for the evaluation of peroxide consumption during photo-Fenton degradation of 2,4-dichlorophenol using blacklight irradiation. (c) 2004 Elsevier B.V. All rights reserved.

Spectrophotometric detection of arsenic using flow-injection hydride generation following sorbent extraction preconcentration

An automated system with a C-18 bonded silica gel packed minicolumn is proposed for spectrophotometric detection of arsenic using flow-injection hydride generation following sorbent extraction preconcentration. Complexes formed between arsenic(III) and ammonium diethyl dithiophosphate (ADDP) are retained on a C-18 sorbent. The eluted As-DDP complexes are merged with a 1.5% (w/v) NaBH4 and the resulting solution is thereafter injected into the hydride generator/gas-liquid separator. The arsine generated is carried out by a stream of N-2 and trapped in an alkaline iodine solution in which the analyte is determined by the arsenomolybdenum blue method. With preconcentration time of 120 s, calibration in the 5.00-50.0 mu g As l(-1) range and sampling rate of about 20 samples h(-1) are achieved, corresponding to 36 mg ADDP plus 36 mg ammonium heptamolybdate plus 7 mg hydrazine sulfate plus 0.7 mg stannous chloride and about 7 mi sample consumed per determination. The detection limit is 0.06 mu g l(-1) and the relative standard deviation (n = 12) for a typical 17.0 mu g As l(-1) sample is ca. 6%. The accuracy was checked for arsenic determination in plant materials from the NIST (1572 citrus leaves; 1573 tomato leaves) and the results were in agreement with the certified values at 95% confidence level. Good recoveries (94-104%) of spiked tap waters, sugars and synthetic mixtures of trivalent and pentavalent arsenic were also found. (C) 1999 Elsevier B.V. B.V. All rights reserved.