Reator de UV-Ozônio com lâmpada a vapor de mercúrio a alta pressão modificada para tratamento superficial de óxidos transparentes condutivos utilizados em dispositivos poliméricos eletroluminescentes

An UV-Ozone reactor was developed with an ignition tube extracted into HID mercury lamp used to irradiation on zinc oxide (ZnO) and fluorinated tin oxide (FTO) films for PLEDs devices. Different exposures times were used. In contact angle measurements revealed better results for ZnO and FTO by 15 and 5 min, respectively. In Diffuse Reflectance Infra-red Fourier Transformed (DRIFT) spectroscopy allowed the observation of water, hydrocarbon and carbon dioxide adsorbed on the untreated TCO surfaces. After the UV-Ozone treatment the contaminants were significantly reduced or eliminated and the PLEDs devices decreased threshold voltages in comparison with respectively untreated TCOs.

Development and validation of a high performance liquid chromatographic method for determination of cyclosporine-A from biodegradable intraocular implants

An HPLC method was developed and validated aiming to quantify the cyclosporine-A incorporated into intraocular implants, released from them; and in direct contact with the degradation products of PLGA. The separation was carried out in isocratic mode using acetonitrile/water (70:30) as mobile phase, a C18 column at 80 ºC and UV detection at 210 nm. The method provided selectivity based on resolution among peaks. It was linear over the range of 2.5-40.0 µg/mL. The quantitation and detection limits were 0.8 and 1.2 µg/mL, respectively. The recovery was 101.8% and intra-day and inter-day precision was close to 2%.

Development and validation of a dissolution test for diltiazem hydrochloride in immediate release capsules

This work describes the development and validation of a dissolution test for 60 mg of diltiazem hydrochloride in immediate release capsules. The best dissolution in vitro profile was achieved using potassium phosphate buffer at pH 6.8 as the dissolution medium and paddle as the apparatus at 50 rpm. The drug concentrations in the dissolution media were determined by UV spectrophotometry and HPLC and a statistical analysis revealed that there were significant differences between HPLC and spectrophotometry. This study illustrates the importance of an official method for the dissolution test, since there is no official monograph for diltiazem hydrochloride in capsules.

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.

Precipitação seletiva de tamanhos em nanopartículas semicondutoras coloidais de CdTe e CdSe: um estudo por espectroscopia UV-VIS

The post-preparative size-selective precipitation technique was applied in CdTe and CdSe semiconductor nanocrystals prepared via colloidal route in water. The synthesis of CdTe and CdSe nanoparticles and the effect of the post-preparative size-selective precipitation have been characterized mainly by mean of ultraviolet and visible absorption spectroscopy (UV-Vis). It was demonstrated that the size-selective precipitation are able to isolate particles of different sizes and purify the nanoparticles as well.

Simultaneous determination of moxifloxacin and H2 receptor antagonist in pharmaceutical dosage formulations by RP-HPLC: application to in vitro drug interactions

Simultaneous determination of moxifloxacin (MOX) and H2-antagonists was first time developed in bulk and formulations. Purospher STAR C18 (250 x 4.6 mm, 5 μm) column was used. The mobile phase (methanol: water: ACN, 60:45:5 v/v/v, pH 2.7) was delivered at a flow rate of 1.0 mL min-1, eluent was monitored at 236, 270 and 310 nm for cimetidine, famotidine and ranitidine, respectively. The proposed method is specific, accurate (98-103%), precise (intra-day and inter-day variation 0.098-1.970%) and linear (r>0.998). The LOD and LOQ were 0.006-0.018 and 0.019-0.005 μg mL-1, respectively. The statistical parameters were applied to verify the results. The method is applicable to routine analysis of formulations and interaction of MOX with H2-antagonist.

Simultaneous spectrophotometric determination of lamivudine and zidovudine in fixed dose combinations using multivariate calibration

The simultaneous determination of two or more active components in pharmaceutical preparations, without previous chemical separation, is a common analytical problem. Published works describe the determination of AZT and 3TC separately, as raw material or in different pharmaceutical preparations. In this work, a method using UV spectroscopy and multivariate calibration is described for the simultaneous measurement of 3TC and AZT in fixed dose combinations. The methodology was validated and applied to determine the AZT+3TC contents in tablets from five different manufacturers, as well as their dissolution profile. The results obtained employing the proposed methodology was similar to methods using first derivative technique and HPLC.

Optimization of a HPLC procedure for simultaneous determination of cisplatin and the complex cis,cis,trans-diamminedichlorodihydroxoplatinum(IV) in aqueous solutions

A RP-HPLC procedure for the simultaneous determination of cisplatin and the complex cis,cis,trans-diamminedichlorodihydroxo-platinum(IV), was development. The developed procedure was validated in terms of linearity, accuracy, precision, limits of detection (LOD), limits of quantification (LOQ) and specificity. The limits of detection (LOD) were 0.47 x 10-4 and 0.53 x 10-4 mol L-1 and the limits of quantification (LOQ) were 1.57 x 10-4 and 1.75 x 10-4 mol L-1, for cisplatin and cis,cis,trans-diamminedichlorodihydroxopla-tinum(IV), respectively. The average recoveries of cisplatin and cis,cis,trans-diamminedichlorodihydroxoplatinum(IV) was 100.6% ± 1.4 and 101.2% ± 1.1, respectively. Intermediate (inter-day) precision, repeatability and specificity of the procedure for hydrolysis products of cisplatin were studied. The results of the study showed that the proposed RP-HPLC procedure is simple, rapid, precise, accurate and specific.

Validação de método analítico por espectrofotometria UV para sistema emulsionado lipídico contendo benznidazol

A validation study of an UV spectrophotometric method was conducted for quantitative analysis of benznidazol (BZN) in a lipid. The analytical determinations were performed at 315 nm at 25 ºC. The emulsion components did not interfere on drug analyses, demonstrating the specificity of the methodology. A good linearity (r = 0.99995) and precision (RSD < 5.0%) for intra and inter-day studies, including the reproducibility test were observed. The accuracy ranged of 102.1 + 2.8 e 103.8 + 1.7%. The statistical analysis demonstrates a linear, precise, accurate and robust method for BZN quantification from the lipid emulsion system.

Characterization of the antibiotic doripenem using physicochemical methods: chromatography, spectrophotometry, spectroscopy and thermal analysis

Doripenem was characterized through physicochemical and spectroscopic techniques, as well as thermal analysis. TLC (Rf = 0.62) and HPLC (rt = 7.4 min) were found to be adequate to identify the drug. UV and infrared spectra showed similar profile between doripenem bulk and standard. The ¹H and 13C NMR analysis revealed chemical shifts that allowed identifying the drug. Thermal analysis demonstrated three steps with mass loss, at 128, 178 and 276 ºC. The work was successfully applied to qualitative analysis of doripenem, showing the reported methods can be used for physicochemical characterization of doripenem

Estudo da decomposição fotoquímica por exposição à luz UV de fotorresinas positivas

Positive photoresists are widely used in lithographic process in microelectronics and in optics for the fabrication of relief components. With the aim of identifying molecular modifications among positive photoresists unexposed and previously exposed to ultraviolet light the electron stimulated ion desorption technique coupled to time-of-flight mass spectrometry was employed in the study of the AZ-1518 photoresist. Mass spectra were obtained as a function of the electron beam energy, showing specific changes related to the photochemical decomposition of the photoresist. This reinforces the applicability of the technique to investigate and characterize structural changes in photosensitive materials.

Development of a simple UV-spectrophotometric method for the determination of lansoprazole and study of its degradation profile

A UV-spectrophotometric method is described for the determination of lansoprazole (LAN). The method is based on the measurement of the absorbance of LAN solution in acetonitrile at 281 nm. The system obeyed Beer's law over the concentration range of 1.25-25.0 µg/mL. The degradation behavior of LAN was investigated under dry heat treatment, UV-degradation, acid hydrolysis, alkali hydrolysis and oxidation; and found to degrade extensively under acid hydrolysis, alkali hydrolysis and oxidation. The method was applied to the determination of LAN in capsule and the results were statistically compared with those of the reference method by applying Student's t-test and F-test.

Performance characteristics of high performance liquid chromatography, first order derivative UV spectrophotometry and bioassay for fluconazole determination in capsules

The bioassay, first order derivative UV spectrophotometry and chromatographic methods for assaying fluconazole capsules were compared. They have shown great advantages over the earlier published methods. Using the first order derivative, the UV spectrophotometry method does not suffer interference of excipients. Validation parameters such as linearity, precision, accuracy, limit of detection and limit of quantitation were determined. All methods were linear and reliable within acceptable limits for antibiotic pharmaceutical preparations being accurate, precise and reproducible. The application of each method as a routine analysis should be investigated considering cost, simplicity, equipment, solvents, speed, and application to large or small workloads.

Photochemical characteristics of diclofenac and its photodegradation of inclusion complexes with β-cyclodextrins

Diclofenac is one of most frequently detected compounds in the water cycle. In this work, the effect of initial concentration, liquid inclusion complexes with β-Cyclodextrins (β-CDs) on the photodegradation of diclofenac were studied. Six phototransformation products were detected by HPLC chromatograms. UV-absorption spectra of diclofenac and phototransformation products were determined. One of the phototransformation products was identified. The degradation followed pseudo-first-order kinetics. The experiment showed that irradiation of diclofenac in the presence of β-CDs increase photodegradation rate and determined the optimal molar ratio of diclofenac to β-CDs as 1:2. The reduced photohaemolytic activity of diclofenac in the presence of β-CDs may be attributed to the sequestering and stabilizing of the radical intermediates and /or photoproducts by complexation.

Identificação de extratos etanólicos de madeiras utilizando seu espectro eletrônico de absorção e análise multivariada

The application of multivariate analysis to spectrophotometric (UV) data was explored for distinguishing extracts of cachaça woods commonly used in the manufacture of casks for aging cachaças (oak, cabreúva-parda, jatobá, amendoim and canela-sassafrás). Absorbances close to 280 nm were more strongly correlated with oak and jatobá woods, whereas absorbances near 230 nm were more correlated with canela-sassafrás and cabreúva-parda. A comparison between the spectrophotometric model and the model based on chromatographic (HPLC-DAD) data was carried out. The spectrophotometric model better explained the variance data (PC1 + PC2 = 91%) exhibiting potential as a routine method for checking aged spirits.