Quantitative analysis of phenol and alkylphenols in Brazilian coal tar

The main purpose of this work is the identification and quantification of phenolic compounds in coal tar samples from a ceramics factory in Cocal (SC), Brazil. The samples were subjected to preparative scale liquid chromatography, using Amberlyst A-27TM ion-exchange resin as stationary phase. The fractions obtained were classified as "acids" and "BN" (bases and neutrals). The identification and quantification of phenols, in the acid fraction, was made by gas chromatography coupled to mass spectrometry (GC/MS). Nearly twenty-five phenols were identified in the samples and nine of them were also quantified. The results showed that coal tar has large quantities of phenolic compounds of industrial interest.

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.

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.

Identification of acetates in elasmopalpulus lignosellus pheromone glands using a newly created mass spectral database and kóvats retention indices

Based on a specially created mass spectral database utilizing 23 tetradecenyl and 22 hexadecenyl acetate standards along with Kóvats retention indices obtained on a very polar stationary phase [poly (biscyanopropyl siloxane)] (SP 2340), (Z)-9-hexadecenyl acetate, (Z)-11-hexadecenyl acetate and (E)-8-hexadecenyl acetate were identified in active pheromone extracts of Elasmopalpus lignosellus. This identification was more efficient than our previous study using gas chromatography/mass spectrometry with a dimethyl disulfide derivative where we could only identify the first two acetates. The acetate composition of the pheromone gland differed from region to region in Brazil and from that from the Tifton (GA, USA) population, suggesting polymorphism or a different sub-species.

Validação de método por cromatografia líquida de alta eficiência para determinação da lamivudina e zidovudina em comprimidos

An HPLC method was validated to assay lamivudine and zidovudine combined in tablets. The chromatographic separation was carried out using methanol and acetate buffer pH 6.5 (50:50 v/v) and a RP-18 column, as mobile and stationary phase, respectively. The UV detection was at 270 nm. The method was linear in the range of 24 - 36 µg/mL (lamivudine) and 48 - 72 µg/mL (zidovudine). The recovery (accuracy) ranged from 101.35% to 103.04% and the precision (repeatability and intermediate precision) was less than 2%. The method can be also applied to the quantification of these drugs in the dissolution test of tablets containing both drugs.

Um espalhador de baixo custo de fase estacionária em placas para cromatografia em camada delgada

Chromatography is a means of separating mixtures into their several components. TLC, mainly a liquid/solid process, is one of the separation techniques most often used. It is indispensable in laboratories dealing with natural products, organic and analytical chemistry. Commercial chromatography plates are offered at relatively high cost. In this work the construction of a hand-operated plate coater of stationary phases of low cost and good reproducibility is described to be used in teaching laboratories and research.

Construção de câmara de luz ultravioleta para fotopolimerização de fases estacionárias monolíticas

The assembly of a photochemical reactor with six fluorescent lamps, used for photopolymerizations is described. This chamber presents a mobile support, allowing the placement of samples at different heights and a safety lock that interrupts the radiation, if it is opened during operation. The mirrored internal walls avoid the dispersion and non-uniform distribution of light. There is no high heating because the own character of the used lamps. All parts could be purchased in commerce with less than U$ 150,00. This reactor was successfully used for monolithic stationary phase photopolymerization.

Desenvolvimento de métodos analíticos para determinação de agrotóxicos em sedimentos por cromatografia gasosa monodimensional e bidimensional abrangente com micro detector de captura de elétrons

The development of analytical methods for determination of eight pesticides of different chemical classes (trichlorfon, propanil, fipronil, propiconazole, trifloxystrobin, permethrin, difenoconazole and azoxystrobin) in sediments with gas chromatography-micro-electron capture detector (GC/µECD) and comprehensive two-dimensional gas chromatography with micro-electron capture detector (GCxGC/µECD) is described. These methods were applied to real sediment samples, and the best results were obtained using a 5% diphenyl-methylpolysiloxane column for 1D-GC. For GCxGC the same column was employed in the first dimension and a 50%-phenyl-methylpolysiloxane stationary phase was placed in the second dimension. Due to the superior peak capacity and selectivity of GCxGC, interfering matrix peaks were separated from analytes, showing a better performance of GCxGC.

Possibilidades e limitações no uso da temperatura em cromatografia líquida de fase reversa

High-temperature liquid chromatography (HTLC) is a technique that presents a series of advantages in liquid phase separations, such as: reduced analysis time, reduced pressure drop, reduced asymmetry factors, modified retentions, controlled selectivities, better efficiencies and improved detectivities, as well as permitting green chromatography. The practical limitations that relate to instrumentation and to stationary phase instability are being resolved and this technique is now ready to be applied for routine determinations.

Fases estacionárias modernas para cromatografia líquida de alta eficiência em fase reversa

This review first discusses the limitations of many of the supports and stationary phases used in reversed phase high performance liquid chromatography and then describes those, developed more recently, that present better stabilities and more versatile selectivities. Emphases will be given to stationary phases that use higher purity silicas, hybrid silicas, monolithic silicas, metallic oxides and mixed oxides as supports and those that have embedded polar groups or contain phenyl or fluoro groups as the stationary phase as well as the phases used for mixed mode or hydrophilic interaction separations. These modern stationary phases facilitate the analysis of complex mixtures.

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.

Investigando cinza da casca do arroz como fase estacionária em cromatografia: uma proposta de aula experimental nos cursos de graduação

This article describes an experiment that involves the extraction and separation of the pigments of spinach extract by column chromatography using the silica obtained from rice husk ash as a stationary phase. The experimental procedure is very simple to apply in the chemistry laboratory, and allowed to illustrate some concepts of organic chemistry: structure of organic molecules, solubility, polarity, extraction, partition coefficient, adsorption and retention factor (Rf), as well as objectives and fundamentals of chromatographic methods. The experiment can be carried out in a 4 h period.

O desafio de analisar solutos básicos por cromatografia líquida em modo reverso: algumas alternativas para melhorar as separações

This review considers some of the difficulties encountered with the analysis of basic solutes using reversed-phase chromatography, such as detrimental interaction with stationary phase silanol groups. Methods of overcoming these problems in reversed-phase separations, by judicious selection of the stationary phase and mobile phase conditions, are discussed. Developments to improve the chemical and thermal stability of stationary phases are also reviewed. It is shown that substantial progress has been made in the manufacturing of stationary phases, enabling their use over a wide variety of experimental conditions. In addition, general measures to significantly extend their lifespan are discussed.

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%.

Preparação, caracterização e aplicação de fases estacionárias tipo C8 modificadas por óxidos metálicos para cromatografia líquida

This work describes three C8-stationary phases for high performance liquid chromatography based on silica metallized with ZrO2, TiO2 or Al2O3 layers, having poly(methyloctylsiloxane) immobilized onto their surfaces. The stationary phases were characterized using XRF, XAS, FTIR, SEM and elemental analysis to determine the physical characteristics of the oxide and polysiloxane layers formed on the surfaces and chromatographically to evaluate the separation parameters. The results show the changes on the silica surface and allowed proposing a structure for the oxide layer, being observed tetrahedral and octahedral structures, what is completely new in the literature. The formation of a homogeneous layer of metallic oxide (TiO2 and ZrO2) was observed on the silica. The C8-titanized and C8-aluminized stationary phases presented good chromatographic performances, with good values of asymmetry and efficiency. All stationary phase presented few loss of the polymeric layer after the HPLC, indicating that this layer is well attached on the metalized support.