Determination of 5-aminosalicylic acid in pharmaceutical formulations by square wave voltammetry at pencil graphite electrodes

An analytical method for the determination of the anti-inflammatory drug 5-aminosalicylic acid (5-ASA) in pharmaceutical formulations using square wave voltammetry at pencil graphite electrodes was developed. After the optimization of the experimental conditions, calibration curves were obtained in the linear concentration range from 9.78 × 10-7 to 7.25 × 10-5 mol L-1 resulting in a limit of detection of 2.12 ± 0.05 x 10-8 mol L-1. Statistical tests showed that the concentrations of 5-ASA in commercial tablets and enemas obtained with the proposed voltammetric method agreed with HPLC values at a 95% confidence level.

Validação de método para a determinação de 5-hidroximetilfurfural em mel por cromatografia líquida e sua influência na qualidade do produto

In honey 5-hydroxymethyl-2-furaldehyde (HMF) is one of the most typical products of degradation: it is usually absent in fresh honey, but its concentration tends to rise as a result of heating processes or long-term storage. The validation protocol was performed in terms of detection and quantification limits, precision (by repeatability and intermediate precision), linearity and accuracy (by recovery tests). The method has been tested on 15 honey samples of different ages and geographical origin. HMF correlated highly with the age of the samples has been considered a very important parameter to put these honeys on the market or not and/or to estimate their shelf life.

The syntheses of the marine metabolites 3-bromoverongiaquinol and 5-monobromocavernicolin

An efficient synthesis of the marine metabolite 3-bromoverongiaquinol (1) and the first total synthesis of 5-monobromocavernicolin (2), both isolated from the marine sponge Aplysina cavernicola, have been described based on the 1,2 addition of the lithium enolate of N,O-bistrimethylsilylacetamide (BSA, 4) to 1,4-benzoquinone (3). Bromination and purification of the crude product on silica gel chromatography provided 3-bromoverongiaquinol (1) in 50% overall yield. Under alkaline conditions, the crude product of the bromination reaction was converted to 5-monobromocavernicolin (2) in 20% yield which was also obtained in 13% yield (25% yield based on recovered starting material) from 3-bromoverongiaquinol (1).

Síntese de 5-nitro-isatina e 5-cloro-isatina a partir da isonitrosoacetanilida

This article describes the preparation of 5-nitroisatin and of 5-chloroisatin from isonitrosoacetanilide in a single step, using readily available and inexpensive reagents. These reactions require around 90 minutes and may be carried out as an undergraduate experiment, providing an opportunity to discuss the electrophilic aromatic substitution mechanism, as well as spectroscopic techniques for product identification.

Determinação de 2,5-hexanodiona em urina empregando cromatografia líquida de alta eficiência, após derivatização com 2,4-dinitrofenil-hidrazina

A method for quantifying urinary 2,5-hexanedione was optimized and validated. Urine samples were hydrolyzed and derivatized with 2,4-dinitrophenylhydrazine. The analyte was separated in a high performance liquid chromatography system with a diode array detector, using a C18 column (150 x 4.6 mm, p.d. 5 µm) and a mobile phase composed of phosphate buffer pH 2.3:acetonitrile (40:60, v/v), at a flow rate of 1 mL/min. The chromatograms were monitored at 334 nm. Retention time was 7.3 minutes. Main validation parameters were: coefficient of determination: 0.9994, accuracy: 96 to 107%; intra-assay precision (RSD): 3.08 to 6.72%; inter-assay precision (RSD): 2.54 to 8.17% and limit of quantitation of 0.19 µg/mL.

Synthesis and biological activity of n-{5-(4-methylphenyl) diazenyl-4-phenyl-1, 3-thiazol-2-yl}benzamide derivatives

In the present study, various amides of 2-amino-5-(4-methylphenyl)-diazenyl-4-phenyl-1, 3-thiazole was synthesized and their biological activities were evaluated. All the synthesized compounds were characterized by the combination of elemental analysis and standard spectroscopic methods. They are screened for anti-bacterial activity against Escherichia coli and Staphylococcus aureus as well as screened for antifungal activity against Aspergillus niger and Apergillus oryzae by cup plate method at 1 µg/ mL concentration in DMF.

Caracterización de la biomasa inactiva de Aspergillus niger O-5 como sorbente de Pb (II)

The inactive biomass of fungus Aspergillus niger O-5 obtained in Cuba was characterized as sorbent of Pb2+ by several structural analysis and others techniques. In addition, the biomass was studied for the separation / preconcentration of Pb2+ from aqueous solution. The maximum biosorption capacity was obtained for the contact time of 30 min and pH 5. The kinetic of sorption process occurred according to the model of Ho. The Freundlich or Langmuir models suitably described the experimental adsorption isotherms. The biomass can be used as sorbent for Pb2+ with a maximum capacity of 4.7 - 6.2 mg g-1. The pretreatment with NaOH solution improved its sorption capacity.

Synthesis, antimicrobial and cytotoxic activities of 5-benzylidene-2-[(pyridine-4-ylmethylene)hydrazono]-thiazolidin-4-one and 2-[(pyridine-4-ylmethylene) hydrazono]-thiazolidin-4-one derivatives

A new series of 5-benzylidene-2-[(pyridine-4-ylmethylene)hydrazono]-thiazolidin-4-ones 4a-l have been synthesized. These compounds were designed by a molecular hybridization approach. 2-[(Pyridine-4-ylmethylene)hydrazono]-thiazolidin-4-ones 3a-d were also obtained and used as intermediates to give the target compounds. The in vitro antimicrobial and cytotoxic activities were evaluated for both series. The intermediate 3b showed considerable antibiotic activity against B. subtilis and C. albicans. In the cytotoxic activity compounds 3b (IC50= 4.25 ± 0.36 µg/mL) and 4l (IC50= 1.38 ± 0.04 µg/mL) were effective for inhibition of human erythromyeloblastoid leukemia (K-562) and human lung carcinoma (NCI-H292) cell lines, respectively.

Síntese e caracterização de copolímeros de cadeia lateral derivados de acrilatos de 4,5-di-hidroisoxazol e do (-)-mentol

Five monomers 5-[4-(5-cyano-4,5-dihydroisoxazol-3-yl)phenoxy]undecyl acrylate (7a); n-alkyl 3-{4-[5-(acryloyloxyundecyl)oxyphenyl]}-4,5-dihydroisoxazole-5-carboxylate (7b,c for n-butyl and n-hexyl, respectively); 3-{4-[5-(acryloyloxyundecyl) oxyphenyl]}-4,5-dihydroisoxazole-5-carboxylic acid (7d) and (1R,2S,5R)-2-isopropyl-5-methylcyclohexyl acrylate (9) and the corresponding copolymers 10a-d,11 and homopolymers 12 from 7a and 13 from 9 were designed and synthesized. Except for acrylate 9 which is derived from (-)-menthol, all of the monomers belong to the series containing the isoxazoline ring linked to the acrylate unit by a flexible spacer chain of eleven methylene units. They presented low glass temperature and despite birefringence behavior, these copolymers showed no mesomorphic properties.

Geração de mesoporos em zeólitas ZSM-5 e seus efeitos na conversão do etanol em olefinas

Developing mesoporosity in HZSM-5 zeolites is an alternative for improving their catalytic performance on chemical reactions. In this work, alkaline and thermal treatments were used to produce mesoporosity. These treatments increased mesoporous area and volume. They also influenced the acid properties of the samples. Concerning catalytic performance, treatments modified reaction product distribution. Whereas alkaline treatment favored formation of olefins and increased propene ratio in the beginning of the reaction, thermal treatment resulted in formation of only ethylene due to the low acidity of the sample.

Extração/pré-concentração de íons cobre no ponto nuvem explorando a formação de complexos com DMIT [4,5-dimercapto-1,3-ditiol-2-tionato]

The present study proposes a method for cloud point preconcentration of copper ions at pH 2.0 based on complexes formed with [4,5-dimercapto-1,3-dithyol-2-thionate] and subsequent determination by flame atomic absorption spectrometry (FAAS). Under optimal analytical conditions, the method provided limits of detection of 0.84 and 0.45 µg L-1, by preconcentrating 12.0 and 24.0 mL of sample, respectively. The method was applied for copper determination in water samples, synthetic saliva, guarana powder, tea samples and soft drinks and the accuracy was assessed by analyzing the certified reference materials Dogfish Liver (DOLT-4) and Lobster Hepatopancreas (TORT-2).

Teores de trigonelina, ácido 5-cafeoilquínico, cafeína e melanoidinas em cafés solúveis comerciais brasileiros

Commercial Brazilian regular and decaffeinated instant coffees (33 brands) were studied. The levels ranged from 0.47 to 2.15 g 100 g-1 for trigonelline, 0.38 to 2.66 g 100 g-1 for 5-caffeoylquinic acid (5-CQA), 0.24 to 4.08 g 100 g-1 for caffeine, and 0.253 to 0.476 (420 nm) for melanoidins. Variations in bioactive compound levels among batches were observed. There was no relationship between the drying process and the composition of the products. In general, Gourmet and decaffeinated coffees had higher trigonelline and 5-CQA but lower caffeine and melanoidin content than regular products.

Straightforward synthesis of 2,2,4,4,5,7,7-d7-cholestane: a new deuterated standard in petroleum analysis

A short and efficient synthesis of heptadeuterated 2,2,4,4,5,7,7-d7-cholestane (1) from cholesterol (3) is described. The deuterated material will be useful for the analysis of different sources of petroleum in analytical geochemistry laboratories as internal standard for quantification of steranes via gas chromatography-mass spectrometry (GC-MS).

Autoagregação da 5,10,15,20-tetrakis(4-metoxifenil)porfirina (tmpp): estudos espectroscópicos e análises multivariadas

In this work, the spectroscopic properties of 5,10,15,20-tetrakis(4-methoxyphenyl)porphyrin (TMPP) in solvents of different polarities and water/ethanol mixtures were studied by electronic absorption spectroscopy and resonance light scattering associated with statistical analysis. The molar absorption coefficient and emission maximum of TMPP were dependent on solvent polarity. In the water/ethanol mixture, TMPP remained monomeric up to 25% of water, when it reaches its critical aggregation percentage. Oblique head-to-tail aggregate was found at intermediate water content (35 - 55%), while formation of a J-type aggregate was observed at higher water content (> 60%).

Equilibrium studies of 2,2'-(5-bromo-6-methylpyrimidine-2,4-diyl)bis(azanediyl)dipropanoic acid with some transition-metal ions in aqueous solution

The stability constants of the 1:1 complexes formed between M2+ (M2+: Mn2+, Ni2+, Cu2+, or Cd2+) and BMADA2- (BMADA: 2,2'-(5-bromo-6-methylpyrimidine-2,4 diyl)bis(azanediyl)dipropanoic acid) were determined by potentiometric pH titration in aqueous solution (I = 0.1 mol L-1, NaNO3, 25 °C). The stability of the binary M - BMADA complexes is determined by the basicity of the carboxyl or amino groups. All the stability constants reported in this work exhibit the usual trend, and the order obtained was Mn2+< Ni2+ < Cu2+ > Cd2+. The observed stability order for BMADA approximately follows the Irving - Williams sequence. In the M - BMADA complexes, the M ion is able to form a macrochelate via the pyrimidine group of BMADA.