Development of instrumentation for amperometric and coulometric detection using ultramicroelectrodes

In this work it is presented the development of a simple, portable and inexpensive instrumentation for amperometric and coulometric detection in different analytical instrumentation systems utilizing ultramicroelectrodes. The software, developed in LabVIEW 7.1TM, is capable to carry out three main detection techniques (amperometric, pulsed amperometric and coulometric detection) and a voltammetric technique (cyclic voltammetry). The instrumentation was successfully evaluated using the following systems: cyclic voltammograms of metallic electrodes in alkaline solutions, flow electrochemical detection of glucose and glycine and direct determination of herbicide glyphosate (electrochemical detection coupled to HPLC).Neste trabalho é apresentado o desenvolvimento de uma instrumentação simples, portátil e de baixo custo para detecção amperométrica e coulométrica usando ultramicroeletrodos em diferentes sistemas analíticos. O programa, desenvolvido em LabVIEW 7.1TM, é capaz de realizar três modos de detecção (amperométrico, coulométrico e amperométrico pulsado) e voltametria cíclica. A instrumentação desenvolvida foi avaliada utilizando os seguintes sistemas: voltametria cíclica de eletrodos metálicos em solução alcalina, detecção eletroquímica em fluxo de glicose e glicina, e também na determinação direta do herbicida glifosato (detecção eletroquímica aliada à cromatografia líquida de alta eficiência, CLAE)

Validation of a liquid chromatography ultraviolet method for determination of herbicide diuron and its metabolites in soil samples

ABSTRACT Diuron is one of the most widely herbicide used worldwide, which can undergo degradation producing three primary metabolites: 3,4-dichlorophenylurea, 3-(3,4-dichlorophenyl)-1-methylurea, and 3,4-dichloroaniline. Since the persistence of diuron and its by-products in ecosystems involves risk of toxicity to environment and human health, a reliable quantitative method for simultaneous monitoring of these compounds is required. Hence, a simple method without preconcentration step was validated for quantitation of diuron and its main metabolites by high performance liquid chromatography with ultraviolet detection. Separation was achieved in less than 11 minutes using a C18 column, mobile phase composed of acetonitrile and water (45:55 v/v) at 0.86 mL min-1 and detection at 254 nm. The validated method using solid-liquid extraction followed by an isocratic chromatographic elution proved to be specific, precise and linear (R2 ˃ 0.99), presenting more than 90% of recovery. The method was successfully applied to quantify diuron and their by-products in soil samples collected in a sugarcane cultivation area, focusing on the environmental control

Characterization of intestinal absorption of C-glycoside flavonoid vicenin-2 from Lychnophora ericoides leafs in rats by nonlinear mixed effects modeling

AbstractVicenin-2 (apigenin-6,8-di-C-β-d-glucopyranoside) is present in hydroalcoholic extracts of the Brazilian species Lychnophora ericoides Mart., Asteraceae, leaves, and the biological effects of this compound have been demonstrated including anti-inflammatory, antioxidant and anti-tumor effects in rat models. Given the potential of this compound as a pharmacological agent, the aims of this investigation were to evaluate the extent of intestinal absorption of vicenin-2, and to determine the intestinal permeation profile using an in situ single-pass intestinal perfusion technique. A validated HPLC–UV method was applied to measure the amount of unabsorbed vicenin-2 in the gut after an oral administration of 180 mg kg-1 in five rats. A nonlinear mixed effects model was used to determine the absorption pharmacokinetic parameters assuming a first order absorption and active secretion processes for this compound, wherein the active secretion was characterized by a zero-order process. The population pharmacokinetic parameters obtained were 0.274 min-1 for the first-order absorption rate constant, 16.3% min-1 for the zero-order rate constant; the final percentage of the original dose that was absorbed in vivo was 40.2 ± 2.5%. These parameters indicated that vicenin-2 was rapidly absorbed in the small intestine. In contrast to literature information indicating no absorption of vicenin-2 in Caco-2 cells, our results suggested that vicenin-2 can be absorbed in the small intestine of rats. The finding supports further investigation of vicenin-2 as a viable oral phytopharmaceutical agent for digestive diseases

Development and Validation of a Method for Simultaneous Determination of Bioactive Compounds of Tanacetum parthenium

The sesquiterpene lactones (SL), guaianolide (11,13-dehydrocompressanolide) and parthenolide (4α,5β-epoxy-germacra-1-(10),11-(13)-dien-12,6α-olide), found in Tanacetum parthenium (L.) Schultz Bip, showed in vitro significant activity against Leishmania amazonensis. In this way, a new method for the simultaneous determination of SL was developed and validated. For separation, it was employed high performance liquid chromatography coupled to photodiode array detector (HPLC Alliance e2695-2998PDA, λ 210 nm) with linear gradient of phase (A) acidified water 0.1% H3PO4 (pH 2.8) and phase (B) acetonitrile, in different proportions, at a flow rate of 1.2 mL min-1 with XBridge C8 column (4.6 × 100 mm, 3.5 µm, 35 ºC). The method showed resolution (> 1.5); selectivity, linearity (coefficient of correlation > 0.99), precision (relative standard deviation of 2.2%) and accuracy (recovery > 98%); presenting 52.55 µg mg-1 of guaianolide and 566.05 µg mg-1 of parthenolide in the dichloromethane fraction of the hydroalcoholic extract of Tanacetum parthenium. The method presents potential use in quality control and development of new phytochemicals, a promising alternative in the treatment of leishmaniasis