Determinação da 2,5-hexanodiona em amostras de urina submetidas à hidrólise ácida: importância da coluna cromatográfica e do pH do meio

Acidic hydrolysis of samples is frequent in urinary 2,5-hexanodione determination. This hydrolysis should be performed under proper conditions, in order to avoid interference, such as the presence of 2,5-dimethylfurane and 2-acetylfurane. The results of the present work, as well as data from the literature, show that the use of non-polar or slightly polar chromatographic columns of 30 m length is an essential condition for 2,5-HD determination in an acid hydrolysed urine sample. In the same way the pH should be kept between 0.3 and 0.5. The mean concentrations of 2,5-HD in samples submitted to hydrolysis (0.50 ± 0.28 mg/g of creatinine) was about 3 times higher than those found in the samples without acid hydrolysis (0.19 ± 0.3 mg/g of creatinine).

Aplicação da CLAE para determinação do ácido 10-Hidróxi-2-decenóico (10-HDA) em geléia real pura e adicionada a mel brasileiro

The aim of this paper was to determine the 10-HDA in pure royal jelly and products containing royal jelly, using HPLC methodology. 10-HDA is the natural indicator of the presence of royal jelly in products and also gives the authenticity of pure royal jelly. The chromatographic conditions used were: isocratic system, C18-H column, auto sampler, diode array UV-VIS detector (225 nm), mobile phase with methanol/water (45:55), pH= 2.5 and a-naphtol as internal standard. The results obtained using laboratory samples for pure royal jelly were 2.37%, varying from 0.15% for honey with 10% of royal jelly to 2.10% for honey with 90% of royal jelly respectivelly. For commercial products, the 10-HDA content varied from no detectable to 0.026%. The recovery test presented a minumum of 100.44% The detection limit was 45.92 ng/mL and the quantification limit was 76.53 ng/mL.

Extração de esteróides em frutos de Ottonia martiana Miq., Piperaceae, com gás liqüefeito

A new extraction method for sterols was tested in fruits of Ottonia martiana Miq., a shrub belonging to the family Piperaceae, popularly known as "anestésica" due to the use of its roots and aerial parts, in alcoholic preparations, in treatment of odontological problems. For this purpose, a portable extraction equipment was developed, to operate with liquified gases, which showed to be practical, fast and effective, besides being economical and ecological. In the chromatographic analysis of the extracts obtained in this equipment, it was demonstrated the presence of two sterols, isomers of b-sitosterol and stigmasterol.

O uso de radiação ultravioleta para o pré-tratamento de amostras em análise inorgânica

The basic principles of UV irradiation as sample pre-treatment step and its potential for inorganic analysis are illustrated and discussed through significant examples from the literature. Not only does this overview cover the classical applications of this technique in the decomposition of organic matter in electroanalysis, but it also presents recent trends, including the increasing interest in employing UV irradiation in flow analytical systems, successful attempts to enhance its effectiveness and the coupling with chromatographic and spectroscopic methodologies. Furthermore, a number of relevant cases of UV-driven derivatization reactions involving photo-sensitive inorganic species are presented, showing some convenient options to perform fast and reliable determination of inorganic and organic analytes.

Lignanas de Strychnos guianensis (Aublet) Mart.

The present communication reports the isolation and identification of three lignans from metanolic root extracts of Strychnos guianensis (Aublet) Mart.: olivil (1), cycloolivil (2) and the unknown derivative cycloolivil carbonate (3). From hexane extracts was identified a long chain fatty acid mixture and the triterpene lupeol. The analyses were based on chromatographic and spectroscopy techniques (IR, MS, GC/MS, ¹H-NMR and 13C-NMR, 1D (BB, DEPT 135) and 2D (¹H, ¹ H-COSY, ¹H, 13C-COSY, ¹H, 13C-COSY-LR, HMQC, HMBC and NOESY) and comparison with literature data.

A importância da análise de especiação do chumbo em plasma para a avaliação dos riscos à saúde

Lead absorption is influenced by the species that are formed and the physicochemical characteristics of lead, among others. Lead plasma concentration is < 5% of total blood lead and represents the biologically active fraction able to cross the cell membranes. Health risks mainly depend on a specific metal and its species. Speciation analysis is the analytical activity of identifying and determining different metal species. Chromatographic methods are very useful in the identification of species and the techniques most used to determine metals in biological fluids are ICP OES/MS and AAS. Lead speciation analysis in blood plasma is fundamental for understanding and evaluating the interaction mechanisms between that analyte and its biological targets.

Determination of the HMX and RDX content in synthesized energetic material by HPLC, FT-MIR, and FT-NIR spectroscopies

A new method has been developed for determining the content of mixtures of octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) and hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX), the HMX/RDX ratio, in explosive compositions by Fourier transform infrared spectroscopy (FT-IR), in the regions MIR (mid infrared) and NIR (near infrared) with reference values obtained by chromatographic analysis (HPLC). Plots of relative MIR (A917 / A783) or NIR absorbance values (A4412 / A4317) versus HMX/RDX ratio determined by HPLC analysis revealed good linear relationships.

A simplified procedure for determination of clofentezine residues in fruits by liquid chromatography with UV detection

A rapid and sensitive method is described for the determination of clofentezine residues in apple, papaya, mango and orange. The procedure is based on the extraction of the sample with a hexane:ethyl acetate mixture (1:1, v/v) and liquid chromatographic analysis using UV detection. Mean recoveries from 4 replicates of fortified fruit samples ranged from 81% to 96%, with coefficients of variation from 8.9% to 12.5%. The detection and quantification limits of the method were of 0.05 and 0.1 mg kg-1, respectively.

Cromatografia unificada

The scope of this study encompasses an overview of the principles of unified chromatography as well as the principles of chromatographic techniques as applied to unified systems, which include gas chromatography, liquid chromatography, supercritical fluid chromatography, high temperature and high pressure liquid chromatography, micro-liquid chromatography, enhanced fluidity chromatography, and solvating gas chromatography. Theoretical considerations and individual instrumental parameters such as mobile phase, sample introduction system, columns, and detection system are also discussed. Future applications of this separation approach are discussed.

Validação em métodos cromatográficos e eletroforéticos

The validation of an analytical method is fundamental to implementing a quality control system in any analytical laboratory. As the separation techniques, GC, HPLC and CE, are often the principal tools used in such determinations, procedure validation is a necessity. The objective of this review is to describe the main aspects of validation in chromatographic and electrophoretic analysis, showing, in a general way, the similarities and differences between the guidelines established by the different Brazilian and international regulatory agencies.

Estudo químico e perfil cromatográfico das cascas de Aspidosperma parvifolium A. DC. ("pau-pereira")

Four known alkaloids, uleine, epiuleine, apparicine and desmethyluleine, besides the isoprenoids lupeol and stigmasterol were isolated from the stem bark of Aspidosperma parvifolium. Their identification was based on spectroscopic analysis (UV, IR, ¹H-NMR, 13C-NMR, MS). The chromatographic profile of the ethanolic extract was obtained by HPLC and uleine, epiuleine and apparicine were identified in the extract.

Craqueamento térmico de alcanos: uma aula prática de química orgânica para a graduação

In this work we describe an experiment for the thermal cracking of octane and heptane and the qualitative analyses of the products using the Baeyer test for unsaturated compounds and gas chromatographic analyses. The experiment is very simple and requires one period of two hours and is suitable for undergraduate organic chemistry experimental courses.

Informações essenciais para a caracterização de um sistema de análise em fluxo

Essential aspects for characterization of a flow-based analytical procedure or system are discussed in order to permit the composition of a checklist that will lead to a protocol for reporting results and systems in flow analysis. Aspects more related to chromatographic procedures are not considered. The intent is to present normalized proposals in the field of flow analysis for practitioners and developers.

Diazepam e nordiazepam em plasma: métodos de extração líquido-líquido e em fase sólida no pré-tratamento de amostras para análise cromatográfica em fase líquida

Analysis of diazepam (DZP) and its active metabolite nordiazepam (NDZP) in plasma is commonly performed in clinical medicine to ensure proper therapeutic effects while minimizing the incidence of toxicity. This study aimed to optimize analytical parameters and compare two pre-treatment techniques, liquid-liquid (LLE) and solid phase extraction (SPE), as well as liquid chromatographic conditions to analyze simultaneously DZP and NDZP in plasma from 20 patients treated with a daily dose of 10 mg. Both techniques showed to be well in line with the international criteria for analytical validation, which permitted to quantify DZP (66.2 - 1148.6 ng mL-1) and NDZP (138.5 - 808.6 ng mL -1) in all samples. The correlation coefficients between SPE and LLE were respectively 0.9729 for DZP and 0.9643 for NDZP.

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.