Safety and efficacy indicators of guarana and Brazil nut extract carried in nanoparticles of coenzyme Q10: Evidence from human blood cells and red earthworm experimental model.

This study characterized a nanosupplement based on coenzyme Q10 containing guarana (Paullinia cupana) and Brazil nuts oil (Bertholetia excelsa) (G-Nut). Determined cytotoxic and oxi-immunomodulatory effects on human peripheral blood mononuclear cells (PBMCs) and its effect on mortality of red Californian earthworms (Eisenia fetida) and on the immune efficiency of its coelomocytes immune by in vitro exposure to yeast dead microorganism. The cytotoxic and immunomodulatory effects of G-Nut and the GN-Free extract (0.25-3 mg/mL) were determined in PBMC cultures. Apoptotic, oxidative, and inflammatory markers were determined using biochemical, immunological, and molecular protocols. The effects of G-Nut and GN-Free extracts on mortality and immune efficiency were investigated in earthworms. G-Nut and GN-Free did not induce cytotoxic events in PBMCs, triggering the decrease in apoptotic (caspases 3 and 8) gene expression, lipid and protein oxidation levels, or pro-inflammatory cytokine levels. G-Nut and GN-Free did not trigger earthworm mortality and improved coelomocyte immune efficiency by increasing Eisenia neutrophil extracellular DNA traps and brown body formation when exposed to dead yeasts. The G-Nut nanoformulation is safe and can be used as a new form of food supplement by oral or transdermal delivery.

Achyrocline satureioides infusion, popularly prepared and consumed, has an in vitro protective effect on human neural cells exposed to rotenone.

ETHNOPHARMACOLOGICAL RELEVANCE: Traditional harvest of Achyrocline satureioides (AS) occurs at dawn on Good Friday in some South American countries. Inflorescences are traditionally used as infusions for several disorders, including neuropsychiatric disorders. Pillows and cushions are popularly filled with AS to attenuate the symptoms of depression, anxiety, and sleep disturbances. However, evidence for the potential beneficial effects of AS on human neural cells remains unclear. AIM OF THE STUDY: An in vitro model of SH-SY5Y human neural cells was applied to evaluate the effect of AS infusion, prepared as commonly used, on cells exposed to rotenone and to investigate its potential for neuropsychiatric disorders. MATERIALS AND METHODS: A hot aqueous extract was obtained from a traditionally prepared AS inflorescence infusion and chemically characterized by high-resolution mass spectrometry and spectrophotometric quantification of total polyphenols, tannins, and flavonoids. The SH-SY5Y cell cultures were treated with AS extract at concentrations of 1, 3, 5, 10, 50, 100, and 300 µL/mL to determine the potential cyto- and genotoxic effects of AS on neural cells using MTT, Neutral Red, and GEMO assays. Apoptosis modulation was assessed using flow cytometry and apoptosis-modulating genes were evaluated by qRT-PCR. The protective effect of AS on the neurotoxicity triggered by rotenone exposure (30 nM) was determined by analyzing cellular viability and oxidative markers such as lipid peroxidation and protein carbonylation, and DNA damage was assessed by micronucleus assay. RESULTS: The AS extract, as traditionally prepared, had estimated concentrations of 409.973 ± 31.107 µg/mL, 0.1041 ± 0.0246 mg GAE/mL, and 63.309 ± 3.178 mg QE/mL of total tannins, total polyphenols, and flavonoids, respectively. At concentrations of 30 and 100 µl/mL, AS decreased apoptotic events, whereas the highest concentration (300 µl/mL) increased apoptosis compared to that in the control (p < 0.05). In cells exposed to rotenone, AS treatment induced cell proliferation, reduced DNA damage (as evaluated by micronuclei), and reduced lipid and protein oxidation. CONCLUSIONS: The data indicate the non-cytotoxic and beneficial effects of AS extract on human neural cells by reducing cellular mortality and oxidative stress in neural cells triggered by rotenone exposure.

Recovery of Ce and La from phosphogypsum leachate by adsorption using grape wastes.

The present research aimed to evaluate the use of grape stalk in the adsorption of lanthanum and cerium to identify the best operating conditions enabling the application of the bioadsorbent in REEs leached from phosphogypsum. The grape stalk was characterized and showed an amorphous structure with a heterogeneous and very porous surface. Also, it was possible to identify the groups corresponding to carboxylic acids, phenols, alcohols, aliphatic acids, and aromatic rings. The pH effect study showed that the adsorption process of La3+ and Ce3+ ions was favored at pH 5.0. The adsorption kinetics followed the pseudo-second-order model. In just 20 min, 80% saturation was reached, while equilibrium was reached after 120 min. The adsorption isotherms were appropriately adjusted to the Langmuir model, and the maximum adsorption capacities were obtained at 298 K, which were 35.22 mg g-1 for La3+ and 37.99 mg g-1 for Ce3+. Furthermore, the adsorption process was favorable, spontaneous, and exothermic. In the study's second phase, phosphogypsum was leached with a sulfuric acid solution. Then, the adsorption of REEs was carried out under the experimental conditions of pH after leaching and pH 5.0 (adjustment carried out with sodium hydroxide solution) at 298 K for 120 min and with adsorbent dosages of 1 and 5 g L-1. This process resulted in removal percentages above 95% for the most abundant REEs, such as neodymium, lanthanum, and cerium, at pH 5.0 and a dosage of 5 g L-1, demonstrating the effectiveness of the bioadsorbent used. These results indicate the potential of using grape residue as a promising bioadsorbent in recovering rare earth elements from phosphogypsum leachate.

Interactions Between Calcium Hypochlorite and Irrigants Commonly Used in Endodontic Practice: A Chemical Analysis.

INTRODUCTION: This study aimed to identify possible products resulting from chemical interactions between calcium hypochlorite (Ca[OCl]2) and other irrigants for endodontic use using electrospray ionization quadrupole time-of-flight mass spectrometry. METHODS: The 5.25% Ca(OCl)2 was associated with either 70% ethanol solution, distilled water, saline solution (0.9% sodium chloride), 5% sodium thiosulfate, 10% citric acid, 17% ethylenediaminetetraacetic acid (EDTA), or 2% chlorhexidine (CHX). The reaction ratio was 1:1 and the products obtained were analyzed by electrospray ionization quadrupole time-of-flight mass spectrometry. RESULTS: The interactions between Ca(OCl)2 and CHX generated an orange-brown precipitate, without identification of para-chloroaniline and between Ca(OCl)2 and sodium thiosulfate, a milky-white precipitate. Furthermore, when the oxidizing agent was associated with EDTA and citric acid, chlorine gas was released. As for the other associations, 70% ethanol, distilled water, and saline solution, no precipitation or gas release occurred. CONCLUSIONS: The orange-brown precipitate occurs due to the chlorination of guanidine nitrogens, and the milky-white precipitate is due to the partial neutralization of the oxidizing agent. The release of chlorine gas occurs due to the low pH of the mixture, which results in the rapid formation and decomposition of chlorine. In this context, an intermediate rinsed with distilled water, saline solution, and ethanol between Ca(OCl)2 and CHX, citric acid, and EDTA seems to be appropriate to prevent the formation of by-products when these irrigants need to be used in the canal. Furthermore, if it is necessary to use sodium thiosulfate, a larger volume of the solution must be used compared to that used for the oxidizing solution.

UPLC-ESI/Q-TOF MS/MS Method for Determination of Vildagliptin and its Organic Impurities.

Vildagliptin (VLG) corresponds to a drug used for the treatment of diabetes mellitus. This disease requires continuous treatment, and so the control of impurities present in it is important to assure the quality of this drug. Thus, it is necessary to use sensitive and selective detection techniques and the ultra-performance liquid chromatography is a better option compared with high-performance liquid chromatography because it enhances the separation efficiency with a shorter analysis time and an increased resolution. This research analysis was accomplished by using liquid chromatography/tandem mass spectrometry, and the quantification was performed by using an extracted ion from the VLG drug and its main organic impurities of synthesis. During the validation process, following international standards, the method proved to be linear for the tree substances (R2 = 0.997-0.998) and the analysis of variance showed a non-significant linearity deviation (P > 0.05). Three critical factors were selected to evaluate method robustness with a full factorial experimental design, and the changes in the parameters were found to be not significant for the quantification of VLG and its impurities. The ultra-performance liquid chromatography-tandem mass spectrometry for the determination of impurities in VLG was precise, accurate and robust proving to be effective for analysis in the pharmaceutical industry and to improve the quality, safety and effectiveness of the new drug developed.

Capillary zone electrophoresis method to assay tipranavir capsules and identification of oxidation product and organic impurity by quadrupole-time of flight mass spectrometry.

Tipranavir (TPV) is one of the most recently developed protease inhibitors (PI) and it is specially recommended for treatment-experienced patients who are resistant to other PI drugs. In this work, a simple and friendly environmental CZE stability-indicating method to assay TPV capsules was developed and two TPV organic impurities were identified by high resolution mass spectrometry (HRMS). The optimized analytical conditions were: background electrolyte composed of sodium borate 50mM, pH 9.0 and 5% of methanol; voltage + 28kV; hydrodynamic injection of 5s (100mbar), detection wavelength 240nm, at 25°C. The separation was achieved in a fused silica capillary with 50µm × 40cm (inner diameter × effective length), using furosemide as internal standard. All the validation parameters were met and the method was specific, even in the presence of degradation products and impurities. Oxidation was indicated as the main degradation pathway among those evaluated in this study (acidic, alkaline, thermal, photolytic and oxidative) and it showed a second order degradation kinetic, under the conditions used in this study. The main oxidation product and an organic impurity detected in the standard were characterized by Q-TOF, and both of them correspond to oxidation products of TPV.

Total sulfur determination in residues of crude oil distillation using FT-IR/ATR and variable selection methods.

Total sulfur concentration was determined in atmospheric residue (AR) and vacuum residue (VR) samples obtained from petroleum distillation process by Fourier transform infrared spectroscopy with attenuated total reflectance (FT-IR/ATR) in association with chemometric methods. Calibration and prediction set consisted of 40 and 20 samples, respectively. Calibration models were developed using two variable selection models: interval partial least squares (iPLS) and synergy interval partial least squares (siPLS). Different treatments and pre-processing steps were also evaluated for the development of models. The pre-treatment based on multiplicative scatter correction (MSC) and the mean centered data were selected for models construction. The use of siPLS as variable selection method provided a model with root mean square error of prediction (RMSEP) values significantly better than those obtained by PLS model using all variables. The best model was obtained using siPLS algorithm with spectra divided in 20 intervals and combinations of 3 intervals (911-824, 823-736 and 737-650 cm(-1)). This model produced a RMSECV of 400 mg kg(-1) S and RMSEP of 420 mg kg(-1) S, showing a correlation coefficient of 0.990.