Development of Electroanalytical Methods Using Different Electrodes for the Determination of Progesterone (P4) in Pharmaceutical Formulations and Human,Cow and Goat Milk

For the determination of progesterone (P4) electroanalytical studies were performed using mercury electrode (HMDE) and screen-printed boron-doped diamond electrode (BDD-SPE). The effects of pH, supporting electrolyte, accumulation potential and time (E_acc, t_acc) were studied in both systems. The optimum conditions were: i) HMDE: pH 7,0; E_acc: −0,1 V and t_acc: 40 s, ii) BDD-SPE: 0,5 mol L⁻¹ H₂SO₄; E_acc: 0,0 V and t_acc: 120 s. Under these conditions, the detection limit was 3.1 μg L⁻¹ for HMDE and 45.6 μg L⁻¹ for BDD-SPE. Both methods were validated and applied in the P4 determination on pharmaceutical formulations and milk samples.     

Hydrazine hydrate: A new reagent for Fmoc group removal in solid phase peptide synthesis

In solid-phase peptide synthesis using the Fmoc/tBu strategy (SPPS-Fmoc/tBu), an orthogonal protection scheme of amino acids is used; specifically, the alpha-amine group is protected by the 9-fluorenylmethyloxycarbonyl (Fmoc) group, which is removed by weak bases, while side chains are protected by groups that are acid labile. We demonstrated that hydrazine hydrate is an efficient reagent for eliminating the Fmoc group in SPPS-Fmoc/tBu. First, experimental conditions were established for Fmoc group removal from Fmoc-Val-OH in solution. It was determined that the Fmoc group was completely removed with 16% hydrazine hydrate in DMF after 60?min at rt. Second, SPPS-Fmoc/tBu using hydrazine hydrate for Fmoc group removal was standardized. The Fmoc group removal was completed using 16% hydrazine hydrate in DMF for 10?min at rt (twice). When the reaction of Fmoc group removal was microwave-assisted, the reaction only required 30?s to efficiently remove the Fmoc group in SPPS-Fmoc/tBu. The method reported here can be routinely used, and it is equivalent to conventional SPPS-Fmoc/tBu methodologies where 4-methylpiperidine or piperidine is used.     

Preparation and characterization of a new series of solid solutions of Bi1−xYxFeO3 (0 < x < 1) from the thermal decomposition of hexacyanoferrates doped with yttrium

Solid solutions of Bi_1?xY_x[Fe(CN)₆]·4H₂O (0?<?x?<?1) complexes were synthesized and characterized. The crystal structures were refined by Rietveld analysis using X-ray powder diffraction data. The complexes of the series crystallized in the orthorhombic system, space group Cmcm. The gradual decrease in cell volume indicates that the substitution of Bi³⁺ by Y³⁺ was appropriately materialized. The thermal behavior was studied by thermogravimetric and differential thermal analysis. A single phase of perovskite-type Bi_1?xY_xFeO₃ powders was obtained by thermal decomposition of the complexes at about 600 °C. The obtained products were identified and characterized by energy-dispersive spectroscopy, Raman and Fourier transform infrared spectroscopy and powder X-ray diffraction. The size and morphology of the complexes and their thermal decomposition products were evaluated by scanning electron microscopy. Thermal analysis showed that the complexes were good intermediaries for the synthesis of high-purity mixed oxides with a uniform particle size of the order of nanometers. To evaluate the effect of doping with yttrium, electrical transport measurements were performed.

     

A Potentiometric and Spectroscopic Study on the Interaction Between Human Immunoglobulin G and Sodium Perfluorooctanoate in Aqueous Solution

The interaction between human immunoglobulin G (IgG) and sodium perfluorooctanate (SPFO) has been characterized by a combination of UV-vis and UV-CD spectroscopies and ion selective electrodes. The study determined that there were true specific unions between SPFO and IgG. The conformational changes at the bulk solution, induced by SPFO, were well characterized by UV-vis and UV-CD spectroscopies. Chemical and thermal unfolding were analysed and the thermodynamic parameters were determined.     

Thermal and oxidative stability of Sacha Inchi oil and capsules formed with biopolymers analyzed by DSC and <Superscript>1</Superscript>H NMR

The oxidative stability of edible oils is an important feature to know due the undesirable changes that can occur in the storage. In this way, the oxidative induction time (OIT) value is an indicative to prevent this effect. The objectives of this study were to evaluate the omega-3 content and kinetic parameters of Sacha Inchi oil (SIO) and capsules that are formed with biopolymers, in addition, there were analyzed with differential scanning calorimetry (DSC) and proton nuclear magnetic resonance (¹H NMR). The SIO and capsules, formed using an emulsion, were analyzed with DSC in an oxygen atmosphere to determine the OIT value in isothermal conditions at 100, 120 and 150 °C. The kinetic parameters (activation energy, pre-exponential factor and z value) of SIO were obtained, and the stability time was predicted at different temperatures. The ¹H NMR spectra enabled us to assess the identification and percentage relative before and after the isothermal DSC oxidation of omega-3 concentration and formation of their oxidized compounds. (E-E)-2,4-Alkadienals were the primary oxidized compound and is strongly correlated with the decrease in omega-3 content. Isothermal DSC is a useful to determine the OIT (min) and kinetic parameters to predict the stability oxidation in different edible oils and thus prevent the inadequate consumption of edible oils oxidized.     

Partition Markov model for multiple processes

In this paper, we analyze the model proposed in García and Londoño¹ in which a set of p-independent sequences of discrete time Markov chains is considered, over a finite alphabet A and with finite order o. The model is obtained identifying the states on the state space A^o where two or more sequences share the same transition probabilities (see also García and González-López²). This identification establishes a partition on {1,…,p}×A^o, the set of sequences, and the state space. We show that by means of the Bayesian information criterion (BIC), the partition can be estimated eventually almost surely. Also, in García and Londoño,¹ it is given a notion of divergence, derived from the BIC, which serves to identify the proximity/discrepancy between elements of {1,…,p}×A^o (see also García et al³). In the present article, we prove that this notion is a metric in the space where the model is built and that it is statistically consistent to determine proximity/discrepancy between the elements of the space {1,…,p}×A^o. We apply the notions discussed here for the construction of a parsimonious model that represents the common stochastic structure of 153 complete genomic Zika sequences, coming from tropical and subtropical regions.     

Sample selection procedure in daily trading volume processes

In this paper, we propose a procedure of selecting samples from a set of samples coming from Markovian processes of finite order and finite alphabet. Under the assumption of the existence of a law that prevails in at least q% of the samples of the collection, we show that the procedure allows to identify samples governed by the predominant law. The approach is based on a local metric between samples, which tends to zero when we compare samples of identical law and tends to infinity when comparing samples with different laws. The local metric allows to define a criterion which takes arbitrarily large values when the previous assumption about the existence of a predominant law does not hold. By means of this procedure, we map similarities and dissimilarities of some Brazilian stocks' daily trading volume dynamic.