Ariadne M. Brondi

Mapping the polymorphic forms of fexofenadine in pharmaceutical tablets using near infrared chemical imaging

This study presents a comparison of partial least squares (PLS) and multivariate curve resolution (MCR-ALS) in the quantification of polymorphic forms I and II of fexofenadine. HCl in pharmaceutical tablets using near infrared chemical imaging (NIR-CI). The PLS model built using a standard normal variate (SNV) pre-processing method resulted in satisfactory fits between the reference and predicted values, with a root mean square error of prediction (RMSEP) for both polymorphic forms below 1.5% (w/w). The MCR-ALS results were obtained using an augmented matrix and SNV pre-processing method. The lack of fit value for decomposition was 0.13%, the correlation coefficient between the pure spectra and the obtained spectral profiles was 99.94% and the RMSEP was below 6% (w/w). The MCR-ALS model efficiently quantified the polymorphic forms and generated distribution maps; however, the PLS model exhibited better recovery of the concentrations.

Pre-equilibrium Emission and α-clustering in Nuclei

The study of nuclear states built on clusters bound by valence neutrons in their molecular configurations is a field of large interest, which is being renewed by the availability of exotic beams: clustering is, in fact, predicted to become very important at the drip-line, where weakly bound systems will prevail. Although for light nuclei at an excitation energy close to the particle separation value there are experimental evidences of such structure effects, this is still not the case for heavier nuclear systems. Many attempts have been done using preformation alpha clustering models, but there is still a lack of experimental data capable to give a direct feedback. In particular, searching for alpha clustering effects in medium mass systems is still a challenge, which can give new hints in this subject. In the past we have studied the reactions 250, 192 and 130 MeV 16O + 116Sn, observing a significant increase in the fast emitted α-particle yield. This effect was ascribed to the presence of preformed a-clusters in the 16O projectile nucleus. In order to investigate these aspects, in a model independent way, a new experimental campaign has been performed with the GARFIELD + RCo set up, to compare results from two different reactions: a double magic a-cluster (16O) and a non-magic α-cluster projectile (19F) at the same beam velocity (16AMeV) have been chosen, impinging respectively on 65Cu and 62Ni targets, thus leading to the same 81Rb* compound nucleus. The angular distributions and the light charged particles emission spectra in coincidence with evaporation residues have been measured and analyzed. The preliminary results of the data analysis and the main features of the theoretical model used for their interpretation are presented.

Differential Scanning Calorimetry and Infrared Spectroscopy Combined with Chemometric Analysis to the Determination of Coffee Adulteration by Corn

Roasted and ground coffee is targeted by fraudulent addiction of products. In this way the determination of contaminants in coffee has economic and nutritional importance. In this study, the coffee adulteration by corn were detected using DSC (differential scanning calorimetry) and FTIR (Fourier transform infrared spectroscopy) coupled to PCA (principal component analysis), and PLS (partial least squares) models. Three different levels of roasted and ground Coffea arabica L. were used to prepare mixtures with roasted and ground corn. The level of adulteration used was between 0.5 to 40% (m/m). It was observed that both DSC and FTIR coupled with PCA are able to discriminate adulterated from unadulterated samples of coffee by corn at levels below 1%. PLS models were built with DSC and FTIR data reaching good correlation between the values of estimated and reference concentrations, with RMSECV (root mean square error of cross-validation) lower than 3.5% for DSC data and 2.7% for FTIR data.

Development and Validation of a Chromatography Method Using Tandem UV/Charged Aerosol Detector for Simultaneous Determination of Amlodipine Besylate and Olmesartan Medoxomil: Application to Drug-Excipient Compatibility Study

A study was carried out to investigate compatibility of amlodipine besylate and olmesartan medoxomil with a variety of pharmaceutical excipients. Both drugs are antihypertensive agents that can be administered alone, in monotherapy, or in pharmaceutical association. The studies were performed using binary and ternary mixtures, and samples were stored for 3 and 6 months at 40°C under 75% relative humidity and dry conditions. For this study, a method based on high-performance liquid chromatography (HPLC) was developed and validated for the simultaneous determination of amlodipine besylate and olmesartan medoxomil in samples from pharmaceutical preformulation studies using diode array detector (DAD) and charged aerosol detector (CAD). The runtime per sample was 10 min with retention time of 7.926 min and 4.408 min for amlodipine and olmesartan, respectively. The validation was performed according to ICH guidelines. The calibration curve presents linear dynamic range from 12 to 250 μg mL−1 for amlodipine and from 25 to 500 μg mL−1 for olmesartan with coefficient of determination (R2 ≥ 0.9908) while repeatability and reproducibility (expressed as relative standard deviation) were lower than 1.0%. The excipients such as corn starch, croscarmellose sodium, magnesium stearate, polyvinyl alcohol, talc, polyvinylpyrrolidone, lactose monohydrate, and polyethylene glycol showed potential incompatibilities after accelerated stability testing.

Quantification of Humic and Fulvic Acids, Macro- and MicroNutrients and C/N Ratio in Organic Fertilizers

ABSTRACT Humic substances are the main responsible for soil conditioning and are one of the major components of the composting product. However, there is still little information about their composition and mechanisms of activity. This study aimed to evaluate quantitatively the humic and fulvic fraction by size-exclusion liquid chromatography and the metal content by atomic absorption spectrometry. The chromatographic method used was efficient for humic and fulvic acids quantitation. Levels of 1.73 ± 0.03 and 1.6 ± 0.5 g kg−1 were found for chicken manure regarding humic and fulvic acids, respectively, and 5.1 ± 0.9 and 1.2 ± 0.1 g kg−1 for peat. The metal contents indicated the need of a mineral enrichment, because only the levels of iron reached the minimum recommended by legislation. It was also observed that evaluated organic fertilizers were in accordance with the specifications established by legislation in relation to carbon and total nitrogen and the pathogen levels.