Determinação rápida de oseltamivir em cápsulas por cromatografia líquida de ultraeficiência com detector por arranjo de diodos

A simple and rapid ultra-performance liquid chromatographic method for determination of oseltamivir in capsules was developed and validated. The mobile phase consisted of 5 mmol/L triethylammonium buffer (pH 3.0) and acetonitrile (70:30, v/v). Separation was performed in a Hypersil Gold® column, with octylsilil as stationary phase (100 x 2.1 mm, p.d. 1.9 µm). Chromatography run time was 1.2 min. The method presented adequate specificity, linearity, precision, ruggedness and accuracy and was adequate for determination of oseltamivir in capsules.

Determinação rápida de fármacos básicos em plasma por cromatografia a gás com detector de nitrogênio e fósforo

A simple and fast method for determination of 40 basic drugs in human plasma employing gas-chromatography with nitrogen-phosphorus detection was developed and validated. Drugs were extracted from 800 µL of plasma with 250 µL of butyl acetate at basic pH. Aliquots of the organic extract were directly injected on a column with methylsilicone stationary phase. Total chromatographic run time was 25 min. All compounds were detected in concentrations ranging from therapeutic to toxic levels, with intermediate precision CV% below 11.2 and accuracy in the range of 92-114%.

Determinação de bussulfano em plasma através de cromatografia líquida de alta eficiência com detector de arranjo de diodos e derivatização com dietilditiocarbamato de sódio

A high performance liquid chromatographic-diode array detection method for the determination of busulfan in plasma was developed and validated. Sample preparation consisted of protein precipitation followed by derivatization with sodium diethyldithiocarbamate and liquid-liquid extraction with methyl-tert-butyl ether. Chromatograms were monitored at 277 nm. Separation was carried out on a Lichrospher RP 18 column (5 µm, 250 x 4 mm). The mobile phase consisted of water and acetonitrile (20:80, v/v). The method presented adequate specificity, linearity, precision and accuracy and allowed reliable determination of busulfan in clinical plasma samples, being applied to three patients submitted to bone marrow transplantation.

Determinação simultânea de topiramato, carbamazepina, fenitoína e fenobarbital em plasma empregando cromatografia a gás com detector de nitrogênio e fósforo

Topiramate and the other frequently co-administered antiepileptic drugs carbamazepine, phenytoin and phenobarbital were determined in 100 µL plasma samples by gas chromatography with nitrogen phosphorus detection (GC-NPD), after a one-step liquid-liquid extraction with ethyl acetate, followed by flash methylation with trimethylphenylammonium hydroxide. Total chromatographic run time was 12.5 min. Intra-assay and inter-assay precision was 2.5-7.3% and 1.6-5.2%, respectively. Accuracy was 100.1-104.2%. The limit of quantitation was 1 µg mL-1 for all analytes, proving suitable for routine application in therapeutic drug monitoring of antiepileptic drugs.

Determinação simultânea de carbamazepina, fenitoína e fenobarbital em sangue seco em papel por cromatografia líquida de alta eficiência

Carbamazepine, phenobarbital and phenytoin were determined in dried blood spots (DBS) by high performance liquid chromatography, after extraction of 8 mm DBS using a mixture of acetonitrile and methanol. Analytes were separated by reversed-phase chromatography, with a run time of 17 minutes. Intra-assay and inter-assay precisions were in the 5.3 to 8.4% and 3.3 to 5.2% ranges, respectively. Accuracy was in the 98.8 to 104.3% range. The method had sensitivity to detect all analytes at levels below minimum therapeutic concentrations. The analytes were stable at 4 ºC and room temperature for up to 12 days and at 45 ºC for 9 days. The method was applied to 14 paired clinical samples of blood serum and DBS.

Uso de diagrama V modificado como relatório em aulas teórico-práticas de química geral

In this article, we present data from a study in practical classes for General Chemistry. To this end, it was proposed to use a modified V diagram to replace traditional reporting. These reports consist of material commonly prepared in the subject, including introduction, materials and methods, results and discussion and conclusions. From the preparation of the modified V, the students were able to establish relationships between the theoretical and methodological aspects necessary for understanding the objects and events studied. Thus, student learning can be evaluated in light of the Theory of Meaningful Learning.

ALCALOIDES ACRIDÔNICOS INIBEM CATEPSINA L E V

Cathepsins represent a class of enzymes that has the primary function of randomly degrading proteins in the lysosomes, although are also involved in different pathologies. The aim of this paper was to evaluate the capacity of acridone alkaloids isolated from Swinglea glutinosa (Rutaceae) to inhibit cathepsin L in vitro . The IC50 values found were in the 0.8-57 µM range and the most promising compounds were alkaloids 1 and 2, with IC50 of 0.9 and 0.8 µM, respectively. Enzyme kinetics revealed that they are reversible competitive inhibitors with respect to the substrate Z-FR-MCA. This small series of acridone alkaloids showed low selectivity for both cathepsins, but represent promising lead candidates for the further development of competitive cathepsin L and V inhibitors.

Contribuciones a la ictiologia: V - VI sobre algunas especies de Gobiidae de la colección del Laboratorio Aragó (Banyuls-sur-mer, Francia) y descripción de un nuevo genero (Austrogobius) sudamericano

En el número V de "Contribuciones a la Ictiologia" se dán normas para el estudio sistemático de los organos ciatiformes, que proporcionaron a los Gobiidae de Europa un medio seguro de ordenación genérica y distinción específica. Se añade el estudio de la colección del Laboratorio Aragó, de Banyuls-sur-mer, Francia. En el número VI de "Contribuciones a la Ictiología" se aloja el Gobiosoma parri Ginsburg en el nuevo gênero Austrogobius De Buen, y se dán las características que lo distinguen, especialmente la distribución de tubos mucosos y geniporos.

Spectroscopic analysis of C80 doping with group III and group V elements using semiempirical PM3 molecular modelling technique

Semiempirical calculations at the level of PM3 of theory were carried out to study the structural and electronic properties of C80 and some of its doped derivatives with the elements of group III and V at the level of PM3 of theory. We have selected these elements to be substituted in the fullerene-C80 cage in order to show the effect of such structural change on the electronic properties of the molecules studied. The theoretical IR spectra, some of physical and chemical properties of the molecules studied are obtained and discussed.

A novel indicator reaction for the catalytic determination of V(V) at ppb levels by the kinetic spectrophotometric method

A novel sensitive and relatively selective kinetic method is presented for the determination of V(V), based on its catalytic effect on the oxidation reaction of Ponceau Xylydine by potassium bromate in presence of 5-sulfosalicylic acid (SSA) as activator. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of Ponceau Xylydine at 640 nm between 0.5 to 7 min (the fixed time method) in H3PO4 medium at 25ºC. The effect of various parameters such as concentrations of H3PO4, SSA, bromate and Ponceau Xylydine, temperature and ionic strength on the rate of net reaction were studied. The method is free from most interferences, especially from large amounts of V(IV). The decrease in absorbance is proportional to the concentration of V(V) over the entire concentration range tested (1-15 ng mL−1) with a detection limit of 0.46 ng mL-1 (according to statistical 3Sblank/k criterion) and a coefficient of variation (CV) of 1.8% (for ten replicate measurement at 95% confidence level). The proposed method suffers few interferences such as Cr(VI) and Hg(II) ions. The method was successfully applied to the determination of V(V) in tap water, drinking water, bottled mineral water samples and a certified standard reference material such as SRM-1640 with satisfactory results. The vanadium contents of water samples were also determined by FAAS for a comparison. The recovery of spiked vanadium(V) was found to be quantitative and the reproducibility was satisfactory. It was observed that the results of the SRM 1640 were in good agreement with the certified value.

Uma sinfonia de autoridades: notas sobre a exegese dos antigos - Plotino, Enéada V, 1 [10], 8-9

Este estudo apresenta a exegese dos Antigos em V, 1 [10], 8-9, mostrando que Plotino estabelece um acordo entre as autoridades mencionadas: todos os Antigos por ele aludidos já conheciam, ainda que de modo implícito e inexato, a doutrina das três naturezas. De modo geral, a imprecisão dos seus predecessores consistia em confundir o Um e o Intelecto. Seguindo passo a passo o argumento de Plotino, tenta-se compreender, especialmente, a função de três dentre os filósofos citados. Primeiro, Platão, considerado o testemunho mais exato das antigas doutrinas. Depois, Aristóteles, contra quem Plotino polemiza, mas que parece servir de modelo para a exegese de alguns dentre os filósofos anteriores a Platão. Finalmente, Ferécides, que encerra uma alusão à doutrina pitagórica e, talvez, também, à tradição mítica.

Paradoxo e natureza no livro V da República

O artigo analisa a primeira onda do livro V da República de Platão, levando em conta a oposição entre opinião (dóxa) e ciência (epistéme), só formulada ao final da terceira onda. Sócrates problematiza a opinião corrente que aceita a diferença de natureza entre homens e mulheres para avançar a ideia de uma natureza humana comum. É essa tese paradoxal que justifica que possam ter uma mesma educação e que, assim, possam desempenhar as mesmas funções, vindo a ser guardiões e governantes da cidade.