Fases estacionárias para cromatografia líquida de alta eficiência em fase reversa (CLAE-FR) baseadas em superfícies de óxidos inorgânicos funcionalizados

Particles of porous silica or other solvent resistent inorganic oxides can be functionalized by aliphatic (e.g., C-8 or C-18) or other groups to give stationary phases for use in reversed phase HPLC. The functionalization can be done by bonding of individual groups to the surface of the support particles, by producing an organic polymeric film from pre-polymers, or by adsorbing/immobilizing pre-formed polymers on the surfaces. These three types of functionalization are reviewed.

Desenvolvimento de um dispositivo de baixo custo para medidas por quimiluminescência

A simple and low cost device (ca. US$ 150) that comprises two photodiodes fixed in lab-made Perspex flow cell is proposed for chemiluminescence measurements. The characteristics of the device (large observation window and reduced thickness) allow maximizing the amount of the emitted radiation detected. A sensitivity improvement of ca. 50 % was observed by employing two photodiodes for signal measurements. The performance of the device was assessed by the oxidation of luminol by hydrogen peroxide, yielding a linear response within the range of 2.50 to 500 µmol L-1 H2O2. The detection limit was estimated as 0.8 µmol L-1 hydrogen peroxide which is comparable with those obtained by using equipments based on photomultipliers.

Determinação de alfa-Tocoferol em alho irradiado utilizando cromatografia líquida de alta eficiência (CLAE)

The effects of 60Co ionizing radiations in doses of 0, 75, 100, 150, 200 and 250Gy on garlic, upon the alpha-tocopherol concentration were studied. The alpha-tocopherol contents were established by high performance liquid chromatography (HPLC), after direct hexane extraction from the garlic samples. The alpha-tocopherol was determined through normal-phase column, and mobile phase was composed by hexane: iso-propyl alcohol (99:01 v/v), with 2mL/min flow rate and fluorescence detector. It is statistically shown that an irradiation dose of up to 150 Gy does not affect the garlic alpha-tocopherol content.

Determinação de compostos de massa molecular alta em folhas de plantas da Amazônia

The fractIons of dichloromethane extracts of leaves from andiroba (Carapa guianensis - Meliaceae), caapi (Banisteriopsis caapi - Malpighiaceae), cocoa (Theobroma cacao - Sterculiaceae), Brazil nut (Bertholletia excelsa - Lecytidaceae), cupuaçu (Theobroma grandiflorum - Sterculiaceae), marupá (Simaruba amara - Simaroubaceae) and rubber tree (Hevea brasiliensis - Euphorbiaceae), were analyzed by HT-HRGC and HT-HRGC-MS. Esters of homologous series of fatty acids and long chain alcohols, phytol, amyrines and tocopherols were characterized. The characterization of the compounds was based mainly in mass spectra data and in addition by usual spectrometric data (¹H and 13C NMR, IR).

Desenvolvimento de um dispositivo para obtenção de monocristais de ligas à base de cobre

This paper describes the drawing, construction and optimization of a device, which can be used to obtain single crystals of different metallic materials with melting point from 550 to 1050 ºC. Components of ease obtaining and of low cost were used. The device was based on the modified Bridgman technique and it was used to obtain single crystals of copper-based alloys. The temperature axial profiles and a difference less then 1% in the temperature between the wall and the center of the ceramic tube in the critical region for obtaining single crystals of good quality indicated that the oven presents a good thermal stability. Single crystals of CuZnAl and CuAlAg alloys of good quality were growth and characterized using optical microscopy and Laüe X-ray back reflection.

Determinação de corantes artificiais por cromatografia líquida de alta eficiência (CLAE) em pó para gelatina

Synthetic dyes were determined by high performance liquid chromatography in 76 samples of regular jelly and diet jelly powders, of several flavors produced by seven different manufacturers. Three sample of each product, from different batches, were analyzed. The same qualitative composition was observed for products of the same flavor from different manufacturers, but the quantitative composition varied markedly from one manufacturer to the other. There were no or few significant differences between batches from a given manufacturer, demonstrating good quality control in the use of these additives by the food industry. None of the samples exceeded the limit stipulated by Brazilian legislation.

Análise química quantitativa para a padronização do óleo de copaíba por cromatografia em fase gasosa de alta resolução

Quantitative GC-FID was evaluated for analysis of methylated copaiba oils, using trans-(-)-caryophyllene or methyl copalate as external standards. Analytical curves showed good linearity and reproducibility in terms of correlation coefficients (0.9992 and 0.996, respectively) and relative standard deviation (< 3%). Quantification of sesquiterpenes and diterpenic acids were performed with each standard, separately. When compared with the integrator response normalization, the standardization was statistically similar for the case of methyl copalate, but the response of trans-(-)-caryophyllene was statistically (P < 0.05) different. This method showed to be suitable for classification and quality control of commercial samples of the oils.

Novas fases estacionárias à base de sílica para cromatografia líquida de alta eficiência

The present work reviews recent advances in the preparation of new reversed phase packing materials such as sterically protected, bidentate, hybrid organic-inorganic and monolithic phases and phases containing embedded polar groups. The bonding chemistry involved in the preparation of these phases as well as their advantages over conventional C8 and C18 reversed phases are discussed. Understanding the reasons behind the development of these newer column packings helps analysts select the best stationary phase for a given application.

Identificação de resíduos de disparos de armas de fogo por meio da técnica de espectrometria de massas de alta resolução com fonte de plasma indutivo

The violence derived from crimes involving firearms represents one of the main concerns of society. For this reason modern techniques have emerged in forensic science to identify suspects at crime scenes. This work describes a methodology to identify residues present in the hands of suspect by using a high resolution inductively coupled plasma mass spectrometry and collection procedure based on ethylenediaminetetraacetic acid (EDTA) solution as a complexing agent in moistened swabs. In order to distinguish real gunshot residues from others types of residues present in the hand of suspect, ternary ratio per cent diagrams were developed for antimony (Sb), barium (Ba) and lead (Pb) detected on the hands of volunteers, before and immediately after shooting tests, revealing a remarkable difference in both situations.

Métodos de preparação de nanopartículas metálicas suportadas em carbono de alta área superficial, como eletrocatalisadores em células a combustível com membrana trocadora de prótons

Fuel cells are attracting much interest as efficient and clean energy conversion devices. The main components of low temperature fuel cells are the electrocatalysts used to promote the anodic and cathodic reactions, which are based on platinum and platinum alloys. These electrocatalysts are normally prepared in the form of metal nanoparticles supported on a conductive material, usually high surface area carbon, to improve catalyst utilization and reduce cost. This work presents and comments some methods used presently to produce these electrocatalysts. The performances of the produced electrocatalysts are compared to that of state-of-the-art commercial E-TEK electrocatalysts.

Análise enantiosseletiva de fármacos: contribuições da cromatografia líquida de alta eficiência e eletroforese capilar

The demand for analytical methods suitable for accurate and reproducible determination of drug enantiomers has increased significantly in the last years. High-performance liquid chromatography (HPLC) using chiral stationary phases and capillary electrophoresis (CE) are the most important techniques used for this purpose. In this paper, the fundamental aspects of chiral separations using both techniques are presented. Some important aspects for the development of enantioselective methods, particularly for the analysis of drugs and metabolites in biological samples, are also discussed.

Análise de fármacos em material biológico: acoplamento microextração em fase sólida "no tubo" e cromatografia líquida de alta eficiência

A new solid phase microextraction (SPME) system, known as in-tube SPME, was recently developed using an open tubular fused-silica capilary column, instead of an SPME fiber, as the SPME device. On-line in-tube SPME is usually used in combination with high performance liquid chromatography. Drugs in biological samples are directly extracted and concentrated in the stationary phase of capillary columns by repeated draw/eject cycles of sample solution, and then directly transferred to the liquid chromatographic column. In-tube SPME is suitable for automation. Automated sample handling procedures not only shorten the total analysis time, but also usually provide better accuracy and precision relative to manual techniques. In-tube SPME has been demonstrated to be a very effective and highly sensitive technique to determine drugs in biological samples for various purposes such as therapeutic drug monitoring, clinical toxicology, bioavailability and pharmacokinetics.

Determinação de lamivudina, estavudina e nevirapina, em comprimidos, por cromatografia líquida de alta eficiência

A high performance liquid chromatography method was developed to quantify lamivudine, stavudine and nevirapine combined in tablets. The separation was carried out in less than 10 min using a phosphate buffer of pH 3.0 and acetonitrile (75:25, v/v) as mobile phase, a LiChrospher ODS column and UV detection at 266 nm. The method was linear over the range of 15-135 µg/mL (lamivudine), 4-36 µg/mL (stavudine) and 20-180 µg/mL (nevirapine). The accuracy ranged from 98.56 to 102.04% and intra-day and inter-day precision was less than 1% for the three drugs. The method showed robustness, remaining unaffected by deliberate variations in relevant parameters.

Metodologia para análise simultânea de ácido nicotínico, trigonelina, ácido clorogênico e cafeína em café torrado por cromatografia líquida de alta eficiência

A reverse phase liquid chromatography method was developed for simultaneous determination of trigonelline, caffeine, nicotinic and chlorogenic (5-CQA) acids in roasted coffee. A gradient of acetic acid/acetonitrile was used as mobile phase and detection was carried out in the UV. The samples were extracted with acetonitrile/water (5:95 v/v) at 80 ºC/10 min. Good recovery (89 to 104%), repeatability and linearity were obtained. Detection limits of 0.01, 0.15, 0.04 and 0.04 mg mL-1 were observed for nicotinic acid, trigonelline, 5-CQA and caffeine. The method, applied to arabica and robusta coffees with different degrees of roasting, was efficient and fast (~35 min) and also allowed identification of cinnamic acids.

Utilização de um monitor de vídeo como fonte de alta tensão para eletroforese capilar

This article describes the use of a conventional CRT monitor as a high voltage power supply for capillary electrophoresis. With this monitor, a 23-kV high voltage with a ripple of 1.32% was observed. The reproducibility of the applied high voltage was evaluated by measuring the standard deviations of peak area and migration time for five consecutive injections of a test mixture containing potassium, sodium, and lithium cations at 50 mmol L-1. The errors were about 2.5% and 0.6% for peak area and migration time, respectively. The maximum current tested was about 180 mA, which covers most capillary electrophoresis applications. This system has been successfully used for several months, maintaining the desired level of performance.