Um novo método simples, fácil e reprodutível, de fase reversa para CLAE, usando uma fase estacionária contendo um grupo polar, uréia, embutido, foi desenvolvido e validado para determinação simultânea de cloridrato de clobutinol (CLO) e succinato de doxilamina (DOX) em xarope. A determinação foi realizada em uma coluna C8 uréia (125 mm x 3,9 mm d.i., 5 µm tamanho de partícula) sintetizada em nosso laboratório (LabCrom). A fase móvel consistiu de mistura de acetonitrila:metanol:tampão fosfato pH 2,5, em eluição por gradiente. O detector por arranjos de diodo (DAD) foi utilizado a 230 nm para CLO e a 262 nm para DOX. O método apresentou precisão adequada, com desvio padrão relativo menor que 1%. A presença de excipientes não interferiu nos resultados obtidos. A exatidão foi realizada pela adição dos padrões dos fármacos ao placebo e valores de recuperação aceitáveis foram obtidos. As curvas analíticas mostraram-se lineares (r² 0,9999 para CLO e 0,9998 para DOX) em uma ampla faixa de concentração (2,4-336 µg mL-1 para CLO e 2,3-63 µg mL-1 para DOX). A solução padrão foi estável por 72 horas a temperatura ambiente. Os parâmetros de validação foram realizados conforme o guia ICH.

A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO) and doxylamine succinate (DOX) in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size) synthetized at the Liquid Chomatography Laboratory (LabCrom) of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5) in the gradient mode. The diode array detector (DAD) was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD) less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX) over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX). The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.

Antimicrobials, among other veterinary drugs, are used worldwide in industry and agriculture to protect animal health and prevent economic loss. In recent years, they have been detected in various environmental compartments, including soil, surface and groundwater and have become a topic of research interest. Emphasizing this class of compounds, this review presents the different pathways which veterinary drugs enter in the environment, in particular contaminate soils. Also are presented regulatory aspects and guidelines, adsorption/desorption and degradation of these compounds in soils and the consequences of its dispersal in the environment.

Em vista da eficiência comprovada da biorremediação na degradação de compostos tóxicos ao ser humano, como o benzeno, tolueno, etilbenzeno e xilenos (BTEX), diversas empresas, principalmente as relacionadas com consultorias e remediação ambiental, têm despertado grandes interesses pela implantação da biorremediação como opção para a reabilitação de áreas contaminadas. Em países desenvolvidos, como os Estados Unidos, Canadá e vários países da Europa, a técnica bioquímica de remediação vem sendo amplamente utilizada em trabalhos que se baseiam, por exemplo, no tratamento de solos contaminados por hidrocarbonetos de petróleo. Porém, ao contrário do que se tem notado nesses países, no Brasil, os projetos de biorremediação ainda estão no campo da teoria, com poucos casos práticos, embora exista uma probabilidade real de expansão. A esse despeito, uma das maiores pertinências dessa revisão é elucidar as vantagens que essa técnica pode oferecer quando é utilizada para a degradação de compostos, como os BTEX, em solos tipicamente brasileiros, cujas características físico-químicas contribuem, em muito, para a degradação desses contaminantes. Nessa conjuntura, pesquisas revelam que os fatores ambientais (como teores de umidade e oxigênio) e a disponibilidade de nutrientes nos solos, além das condições climáticas do Brasil, são bastante adequadas para o emprego dessa técnica. Isso pode trazer como vantagens, ótima relação custo-benefício e maior eficiência na degradação de compostos tóxicos e recalcitrantes frente à maioria das técnicas convencionais de remediação. Em síntese, a presente revisão busca enfocar o estado da arte das técnicas de biorremediação de contaminantes em solos, apresentando as mais atuais e recentes aplicações e inovações, tanto no âmbito nacional quanto no internacional.

In view of the proven efficiency of bioremediation in the degradation of compounds toxic to humans, such as benzene, toluene, ethylbenzene and xylenes (BTEX), several companies, especially those related to remediation and environmental monitoring, have shown enormous interest in the deployment of bioremediation as an option for the rehabilitation of contaminated areas. In developed countries such as the United States, Canada and several European countries, these biochemical remediation techniques have been widely used in work that is based, for example, on the treatment of soil contaminated by petroleum hydrocarbons. However, contrary to what has been done in these countries, in Brazil, bioremediation projects are still mainly theoretical, with few practical cases, but there is a real likelihood of expansion. The more important aim of this review is to indicate the advantages that this technique can offer when it is used for the degradation of compounds such as BTEX in typical Brazilian soils, whose physico-chemical characteristics contribute to the degradation of contaminants. Research shows that environmental factors (such as moisture and oxygen levels) and the availability of soil nutrients, in addition to the climatic conditions in Brazil, are quite suitable for the employment of this technique. They may pose, as an advantage, a favorable cost/benefit ratio and the opportunity for greater efficiency in the degradation of toxic and recalcitrant compounds compared to the majority of conventional remediation techniques. In summary, this review focuses on the state of the art of bioremediation techniques of contaminants in soils, presenting the most current and recent applications and innovations, as reported in the national and international media.

This paper describes the use of pesticides in agriculture. Research has shown that significant quantities of pesticide residues have been found in many types of foods. Thus, an overview is given of pesticide residue determinations in fruits and vegetables, with special attention to apples. The toxicity and the adverse effects possibly caused by the exposure of these compounds are alerting the scientific community to develop studies about the validation of analytical methods for multiresidue pesticide determination in these samples. This review shows that pesticide-residue determination in apples is becoming a very important and challenging issue.

Capillary electrochromatography (CEC) is a separation technique in which the mobile phase flow is based on the application of a voltage across a packed capillary, which generates an electroosmotic flow that transports the analytes along the capillary toward the detector. As it combines the separation mechanisms of high-performance liquid chromatography (HPLC) and of capillary electrophoresis (CE), CEC can be considered a hybrid of HPLC and CE. This review presents some fundamental aspects of CEC and is focused on the instrumental advances of the technique, such as column technology, operation modes and detection systems, presenting recent papers on these topics and some applications and perspectives about CEC.

Ultra Performance Liquid Chromatography (UPLC) retains the same principles as High Performance Liquid Chromatography (HPLC), but uses 1-2.1 mm i.d. columns with sub-2 µm particles. It is considered the newest advance in analytical separation science. The use of these small particles with mobile phases at high linear velocities increases resolution and detectability and decreases analysis time. Thus, the analyses are faster, the solvent volume is smaller, the efficiency is higher and the detectability is 2-3 times higher when compared with HPLC analysis.

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.