Determination of Ni(II) in metal alloys by spectrophotometry UV-Vis using dopasemiquinone

A spectrophotometric method was proposed for Ni(II) determination in alloys using a dopa-semiquinone (L-1) to form [Ni(II)(L1-)3]1-, ε = 9.3 x 10³ L mol-1 cm-1. The optimal conditions for the determination were: wavelength 590 nm, temperature 25 °C, reaction time 45 min and pH 7.5. The Beer's law was obeyed for nickel from 3.33 x 10-5 to 1.78 x 10-4 mol L-1. The method was applied to complex samples, such as inox, nickel-titanium and cobalt-chromium alloys. A study of the potential interferents revealed that Mn was the major interferent. The limit of detection and quantification were 2.88 x 10-5 mol L-1 and 3.06 x 10-5 mol L-1, respectively.

Development and validation of RP-LC and uv spectrophotometric methods to assay bromopride in oral and injectable solutions

A reversed-phase liquid chromatographic (LC) and ultraviolet (UV) spectrophotometric methods were developed and validated for the assay of bromopride in oral and injectable solutions. The methods were validated according to ICH guideline. Both methods were linear in the range between 5-25 μg mL-1 (y = 41837x - 5103.4, r = 0.9996 and y = 0.0284x - 0.0351, r = 1, respectively). The statistical analysis showed no significant difference between the results obtained by the two methods. The proposed methods were found to be simple, rapid, precise, accurate, and sensitive. The LC and UV methods can be used in the routine quantitative analysis of bromopride in oral and injectable solutions.

Losartan potassium dissolution test for drug release evaluation in pharmaceutical capsules using HPLC and UV spectrophotometry

This work describes the development and validation of a dissolution test for 50 mg losartan potassium capsules using HPLC and UV spectrophotometry. A 2(4) full factorial design was carried out to optimize dissolution conditions and potassium phosphate buffer, pH 6.8 as dissolution medium, basket as apparatus at the stirring speed of 50 rpm and time of 30 min were considered adequate. Both dissolution procedure and analytical methods were validated and a statistical analysis showed that there are no significant differences between HPLC and spectrophotometry. Since there is no official monograph, this dissolution test could be applied for quality control routine.

Aplicação de fotólise direta e UV/H2O2 a efluente sintético contendo diferentes corantes alimentícios

Food industries employ a lot of synthetic dyes in their products. Most of these dyes are very stable face to the conventional treatments. This work studied the use of advanced oxidation process (AOP) as an alternative to the conventional ones to degrade a synthetic food effluent (photolysis and UV/H2O2 in continuous reactor). The more efficient process was the UV/H2O2 and it presented decoloration and degradation energetic efficiency values equal to 30.775 kWh m-3 and 269.909 kWh m-3, respectively. The color reduction was 96.4% and COD decrease was 38.56%.

Desenvolvimento e validação de um método analítico simples e rápido por espectroscopia UV para quantificação de aciclovir em matrizes hidrofílicas de liberação prolongada

This work reports the validation of an analytical UV spectrophotometric method to assay acyclovir in hydrophilic matrices (assay and dissolution studies). The method was linear in the range between 2.5-20 µg mL-1, presenting a good correlation coefficient ( r = 0,9999). Precision and accuracy analysis showed low relative standart deviation (< 2.0 %) and a good recoveries percentual (98.9-100 %). The procedure was linear, accurate, and robust. The method is simple and cheap. It does not use polluting reagents and can be applied in dissolution studies, being an adequate alternative to assay acyclovir in hydrophilic matrices tablets.

Adsorption of glyphosate in a forest soil: a study using Mössbauer and FT-IR spectroscopy

We studied the adsorption of glyphosate (GPS) onto soil mineral particles, using FT-IR and Mössbauer spectroscopy. From IR measurements for samples collected under native vegetation of a forest reserve, bands at 1632 and 1407 cm-1 could be attributed to the interaction between the carboxylic group of GPS and structural Al3+ and Fe3+ on the surface of mineral particles; bands at 1075 and 1000 cm-1 were observed only for cultivated soil. Mössbauer spectra for these soils were definitely fitted using a broad central doublet in addition to the magnetic component. This multiple quadrupolar component may be attributed to all non-magnetic Fe3+ contributions, including that of the GPS/Fe3+ complex.

Development and validation of UV spectrophotometric method for determination of levofloxacin in pharmaceutical dosage forms

The objective of this research was to develop and validate an alternative analytical method for quantitative determination of levofloxacin in tablets and injection preparations. The calibration curves were linear over a concentration range from 3.0 to 8.0 μg mL-1. The relative standard deviation was below 1.0% for both formulations and average recovery was 101.42 ± 0.45% and 100.34 ± 0.85% for tablets and injection formulations, respectively. The limit of detection and limit of quantitation were 0.08 and 0.25 μg mL-1, respectively. It was concluded that the developed method is suitable for the quality control of levofloxacin in pharmaceuticals formulations.

UV derivative spectrophotometric method for determination of estradiol valerate in tablets

A derivative UV spectrophotometric method for determination of estradiol valerate in tablets was validated. The parameters specificity, linearity, precision, accuracy, limit of detection and limit of quantitation were studied according to validation guidelines. The first-order derivative spectra were obtained at N = 5, Δλ = 4.0 nm, and determinations were made at 270 nm. The method showed specificity and linearity in the concentration range of 0.20 to 0.40 mg mL-1. The intra and interday precision data demonstrated the method has good reproducibility. Accuracy was also evaluated and results were satisfactory. The proposed method was successfully applied to a pharmaceutical formulation.

Discrimination of native wood charcoal by infrared spectroscopy

Brazil is one of the largest producers and consumers of charcoal in the world. About 50% of its charcoal comes from native forests, with a large part coming from unsustainable operations. The anatomic identification of charcoal is subjective; an instrumental technique would facilitate the monitoring of forests. This study aimed to verify the feasibility of using medium and near infrared reflectance spectroscopy to discriminate native (ipê) from plantation charcoals (eucalyptus). Principal Components Analysis, followed by Discriminant Factorial Analysis formed two different groups indicated by Mahalanobis distances of 40.6 and 80.3 for near and mid infrared, respectively. Validation of the model showed 100% efficacy.

Development and validation of an UV spectrophotometric method for the determination of aliskiren in tablets

For determination of aliskiren in commercial samples, an analytical UV spectrophotometric method was developed and validate according to ICH guideline. The method was linear in the range between 40 and 100 μg mL-1 (r² = 0.9997, n = 7) and exhibited suitable specificity, accuracy, precision, and robustness. It is simple, it has low cost, and it has low use polluting reagents. Therefore, the proposed method was successfully applied for the assay and dissolution studies of aliskiren in tablet dosage forms, and the results were compared to a validated RP-LC method, showing non-significant difference (P > 0.05).

Validação de método espectrofotométrico na região do UV para quantificação de famotidina em cápsulas

This work describes the validation of a method for quantification of famotidine in capsules by UV spectrophotometry using as solvents buffer solution at pH 2.5 and buffer solution at pH 4.5. The results show that the method is practical, selective, accurate, precise and linear from 10.0 to 25.0 µg/mL of famotidine in both solvents. However, a variance analysis showed a lower mean percentage of famotidine when buffer at pH 2.5 is used. This effect was attributed to the instability of famotidine in acidic media. Therefore, the use of pH 4.5 buffer was considered suitable for analysis of famotidine in capsules.

Spectroscopic characterization of schiff base-copper complexes immobilized in smectite clays

Herein, the immobilization of some Schiff base-copper(II) complexes in smectite clays is described as a strategy for the heterogenization of homogeneous catalysts. The obtained materials were characterized by spectroscopic techniques, mostly UV/Vis, EPR, XANES and luminescence spectroscopy. SWy-2 and synthetic Laponite clays were used for the immobilization of two different complexes that have previously shown catalytic activity in the dismutation of superoxide radicals, and disproportionation of hydrogen peroxide. The obtained results indicated the occurrence of an intriguing intramolecular redox process involving copper and the imine ligand at the surface of the clays. These studies are supported by computational calculations.

Desenvolvimento de métodos de análise por CLAE-UV para os antimicrobianos tetraciclina, sulfametoxazol e trimetoprima utilizando materiais à base de sílica como sistemas de pré-concentração

This paper evaluates the adsorption capacity of zirconocene-based silica materials in the pre-concentration of antimicrobians (tetracycline, sulfamethoxazole and trimethoprim) in aqueous medium. These materials were prepared by grafting the zirconocene onto silicas pre-treated at different temperatures. The retention capacity of these materials was evaluated by off line SPE and HPLC-UV and the proposed methodology was validated in ultrapure, tap and river water. The recovery for tetracycline was 72% (in the solid phase A) and, for sulfamethoxazole and trimethoprim was 68 and 95% in the commercial C18, respectively. The target antimicrobians were not detected in the Arroio Dilúvio (Porto Alegre - RS).

Biodegradação de uma mistura de corantes têxteis usando o fungo Ganoderma sp: um estudo cinético

The kinetics of biodegradation by the fungus Ganoderma sp of textile dyes Yellow, Blue and Red Procion were studied in effluents using UV-Vis spectroscopy, Partial Least Squares Regression (PLS) and univariate analysis. The kinetic of the reactions were founded intermediate between first and second orders and the rate constants were calculated. The biodegradation after 72 h at 28 ºC were 33.6, 43.5 and 57.7% for the dyes Yellow, Blue and Red Procion, respectively. The quantitative analysis of the effluent by HPLC method can not be used without previous separation.

Adsorção do corante azul de metileno em partículas de argilominerais: análise dos tamanhos das partículas

Interactions of cationic dye methylene blue (MB) with clay particles in aqueous suspension have been extensively studied. As already known, the number of natural negative charges on the clay modifies significantly the particle sizes dispersed in water and therefore the nature of the interaction with the dye. This work evaluated with UV-Vis spectroscopy method how the clay particle sizes weighted on the adsorption and rearrangement of the dye molecules in aqueous system. The results obtained from light-scattering measurements confirmed that larger particles are found in suspensions containing the high-charged clays as the visible absorption band related to the MB aggregates (570 nm) on these suspensions prevailed.