Sistemas interfaceados de análise por injeção em fluxo e eletroforese capilar (FIA - CE): desafios, aplicações e perspectivas

A review about the state-of-the-art of flow injection analysis (FIA) -- capillary electrophoresis (CE) systems is presented. The basic principles of flow injection and capillary electrophoresis are briefly revised. The main aspects of the FIA-CE hybridization, including advantages and shortcomings, are discussed. Some applications involving all different designs are also presented. This review covers the literature from 1997 up to 2000.

Determinação indireta de N-acetil-L-cisteína por injeção em fluxo empregando Ce(IV) e ferroína

An indirect flow injection spectrophotometric procedure is proposed for the determination of N-acetyl-L-cysteine in pharmaceutical formulations. In this system, ferroin ([Fe(II)-(fen)2]2+) in excess, with a strong absorption at 500 nm, is oxidized by cerium(IV) yielding cerium(III) and [Fe(III)-(fen)2]3+ (colorless), thus producing a baseline. When N-acetyl-L-cysteine solution is introduced into the flow injection system, it reacts with cerium(IV) increasing the analytical signal in proportion to the drug concentration. Under optimal experimental conditions, the linearity of the analytical curve for N-acetyl-L-cysteine ranged from 6.5x10-6 to 1.3x10-4 mol L-1. The detection limit was 5.0x10-6 mol L-1and recoveries between 98.0 and 106% were obtained. The sampling frequency was 60 determinations per hour and the RSD was smaller than 1.4% for 2.2x10-5 mol L-1 N-acetyl-L-cysteine.

Phase diagram and complex patterns in the modeling of the bromate-oxalic acid-Ce-acetone oscillating reaction

Simulations have been carried out on the bromate - oxalic acid - Ce(IV) - acetone oscillating reaction, under flow conditions, using Field and Boyd's model (J. Phys. Chem. 1985, 89, 3707). Many different complex dynamic behaviors were found, including simple periodic oscillations, complex periodic oscillations, quasiperiodicity and chaos. Some of these complex oscillations can be understood as belonging to a Farey sequence. The many different behaviors were systematized in a phase diagram which shows that some regions of complex patterns were nested with one inside the other. The existence of almost all known dynamic behavior for this system allows the suggestion that it can be used as a model for some very complex phenomena that occur in biological systems.

Eletroforese capilar acoplada à espectrometria de massas (CE-MS): vinte anos de desenvolvimento

CE-MS has been increasingly used for analysis of a vast array of compounds. This article reviews the different electrophoretic modes, interfaces and mass analyzers that are commonly used in the CE-MS coupling, as well as the technique advantages and performance characteristics. A large compilation of CE-MS applications is also presented. Therefore, this review is both a guide for beginners and a collection of key references for people who are familiar to the technique. Furthermore, this is the first CE-MS review published in a Brazilian journal and marks the installation of the first two commercial CE-MS units in Sao Paulo State.

Estratégias de pré-concentração em eletroforese capilar (CE): parte 1. Manipulação da velocidade eletroforética do analito

Capillary electrophoresis has become a well-established and routine-based separation technique. It is based on the differences between charged analyte mobility in aqueous or organic electrolytes. Its major limitation is the sensitivity due to small sample injection volumes and the narrow diameter of the capillaries, especially when UV detection is used. There are a number of ways to increase the concentration sensitivity. This report shows some on-line preconcentration strategies to perform it in free solution capillary electrophoresis that are based on manipulation of the analyte electrophoretic velocity during the sample introduction (stacking, field amplification and transient isotachophoresis).

Determination of cetirizine in tablets and compounded capsules: comparative study between CE and HPLC

A capillary electrophoresis (CE) method was developed and validated for determination of cetirizine dihydrochloride in tablets and compounded capsules. The electrophoretic separation was performed in an uncoated fused-silica capillary (40 cm x 50 μm i.d.) using 20 mmol L-1 sodium tetraborate buffer (pH 9.3) as background electrolyte, a hydrodinamic sample injection at 50 mBar for 5 s, 20 KV applied voltage at 25 °C, and detection at 232 nm. The proposed method was compared with the high performance liquid chromatographic (HPLC) method previously validated for this drug, and statistical analysis showed no significant difference between the techniques.

Ce - promoted catalyst from hydrotalcites for CO2 reforming of methane: calcination temperature effect

Ce-promoted Ni-catalysts from hydrotalcites were obtained. The effect of calcination temperature on the chemical and physical properties of the catalysts was studied. Several techniques were used to determine the chemical and physical characteristics of oxides. The apparent activation energies of reduction were determined. Catalytic experiments at 48 L g-1h-1 without pre-reduction in CO2 reforming of methane were performed. The spinel-like phase in these oxides was only formed at 1000 ºC. The reduction of Ni2+ in the oxides was clearly affected by the calcination temperature which was correlated with catalytic performance. The catalyst calcined at 700 ºC showed the greatest activity.

Prochloraz residue levels in ginger submitted to Sportak 450 CE" postharvest treatment

A preliminary study was conducted to determine the residue levels of prochloraz in ginger samples treated with Sportak 450 CE® (prochloraz as active ingredient) under laboratory conditions and cold-storage for 15 days at 10°C and 89% RH. Sampling was carried out at 10 and 15 days after Sportak 450 CE® dip treatment (450 and 900 µg mL-1). Pesticide residues were determined by GCECD. During the study, residue levels in ginger ranged between 3.6 and 10.6 mg Kg-1 for prochloraz.

Complicações maternas associadas à via de parto em gestantes cardiopatas em um hospital terciário de Fortaleza, CE

OBJETIVO: Verificar a associação entre complicações maternas e tipo de parto em gestantes cardiopatas, assim como identificar os possíveis fatores clínicos e obstétricos, implicados na determinação da via de parto. MÉTODOS: Estudo retrospectivo e descritivo analisando prontuários médicos das gestantes cardiopatas internadas em Hospital de Referência terciário no município de Fortaleza, Ceará, no período de 2006 a 2007. A população do estudo incluiu todas as gestantes com diagnóstico anteparto de cardiopatias admitidas para realização do parto e excluiu as gestantes que tiveram o diagnóstico de cardiopatia após o parto, independente da idade e semana gestacional. Utilizou-se um questionário semiestruturado com variáveis demográficas, clínicas e obstétricas. Realizou-se, inicialmente, uma análise descritiva por meio de frequências simples e proporções das variáveis sociodemográficas, clínicas e obstétricas. Em seguida foram analisadas possíveis associações entre os aspectos clínicos, obstétricos e tipo de parto, verificando associação entre complicações maternas e tipo de parto. Para isso, foi aplicado o teste Exato de Fischer, considerando p<0,05 para o estabelecimento da significância estatística. Os dados coletados foram processados e analisados utilizando o software Epi-InfoTM, versão 6.04, Atlanta, USA. RESULTADOS: Foram incluídas 73 gestantes cardiopatas. Dentre as congênitas, a comunicação interatrial foi a mais observada (11,0%) e entre as adquiridas, a estone mitral a mais freqüente (24,6%). A proporção de partos cesáreos foi maior do que entre os vaginais, exceto para mulheres com cardiopatia adquirida. Foi encontrada associação entre tipo de cardiopatia e tipo de parto (p=0,01). Houve 13 complicações maternas (17,8%). Dentre as complicações, dez (76,9%) ocorreram por parto cesáreo e três por via vaginal. Não foi encontrada associação entre complicações maternas e tipo de parto em gestantes cardiopatas (p=0,74). CONCLUSÕES: Não houve associação entre a ocorrência de complicações maternas e a via de parto em gestantes cardiopatas.

CORRELACIÓN ESPACIAL ENTRE MALAS HIERBAS EN UNA PRADERA Y SU RELACIÓN CON LA CONDUCTIVIDAD ELÉCTRICA APARENTE DEL SUELO (CE A )

RESUMEN El objetivo de este trabajo fue evaluar la ecología y la correlación lineal y espacial entre malas hierbas de una pradera y su relación con la conductividad eléctrica aparente del suelo (CEa, mS m-1). La toma de muestras se hizo los días: 23/06/2008 (CEa) y el 24/06/2008 (malas hierbas). Los datos fueron analizados por medio de estadística clásica y de herramientas de geoestadística. La mayoría de los datos presentaron distribución de frecuencia logarítmica, siendo necesaria la utilización del krigeado residual. Se encontraron bajos valores de correlación para las medidas de CEa con las mediciones de malas hierbas en el área de estudio, estando las mismas influidas por el relieve del área. Los mapas de variabilidad espacial mostraron que existía relación entre las malas hierbas y los valores de CEa (CEa-V y CEa-H), principalmente con relación al número de especies de malas hierbas, ya que hay un aumento del número de especies cuando se produce disminución de los valores de CEa. Los mapas de variabilidad espacial para las malas hierbas demuestran la dominancia de ciertas especies y el endemismo de otras.

Composição florística da vegetação de carrasco, Novo Oriente, CE

Foi caracterizada a composição florística da vegetação de carrasco do sul do planalto da Ibiapaba em Novo Oriente, Ceará (5°28’ - 5°43’S e 40°52’ - 40º55’W ; 750-850 m de altitude), ocorrendo em Areias Quartzosas profundas. Foram coletadas 184 espécies, incluindo ervas, cipós, subarbustos, arbustos e árvores, distribuídas em 52 famílias. As famílias com maior número de espécies foram Caesalpiniaceae (17), Fabaceae (16), Euphorbiaceae (15), Myrtaceae (11), Bignoniaceae (10) e Mimosaceae (9). De 102 espécies arbustivas e arbóreas da área estudada, 24 ocorreram em áreas de caatingas e cerrados, 29 em cerrados, 17 em caatinga, uma espécie em mata e 31 foram exclusivas do carrasco. Não foi possível definir se o carrasco é um cerradão degradado ou um tipo próprio de vegetação, sendo necessária para isso a realização de levantamentos em outras áreas similares.

Presence of the RHD pseudogene and the hybrid RHD-CE-Ds gene in Brazilians with the D-negative phenotype

The molecular basis for RHD pseudogene or RHDpsi is a 37-bp insertion in exon 4 of RHD. This insertion, found in two-thirds of D-negative Africans, appears to introduce a stop codon at position 210. The hybrid RHD-CE-Ds, where the 3' end of exon 3 and exons 4 to 8 are derived from RHCE, is associated with the VS+V- phenotype, and leads to a D-negative phenotype in people of African origin. We determined whether Brazilian blood donors of heterogeneous ethnic origin had RHDpsi and RHD-CE-Ds. DNA from 206 blood donors were tested for RHDpsi by a multiplex PCR that detects RHD, RHDpsi and the C and c alleles of RHCE. The RHD genotype was determined by comparison of size of amplified products associated with the RHD gene in both intron 4 and exon 10/3'-UTR. VS was determined by amplification of exon 5 of RHCE, and sequencing of PCR products was used to analyze C733G (Leu245Val). Twenty-two (11%) of the 206 D-negative Brazilians studied had the RHDpsi, 5 (2%) had the RHD-CE-Ds hybrid gene associated with the VS+V- phenotype, and 179 (87%) entirely lacked RHD. As expected, RHD was deleted in all the 50 individuals of Caucasian descent. Among the 156 individuals of African descent, 22 (14%) had inactive RHD and 3% had the RHD-CE-Ds hybrid gene. These data confirm that the inclusion of two different multiplex PCR for RHD is essential to test the D-negative Brazilian population in order to avoid false-positive typing of polytransfused patients and fetuses.