A indústria de processamento químico no Brasil: suas motivações para pesquisa e desenvolvimento e suas interfaces com as políticas governamentais

As the Chemical Science is an experimental one a Chemical Industry require technical people in all its staff level: from Directors and Managers to Operators. This chemical and chemical engineering based education is the foundation of the innovate process and motivation. The paper discusses this and the role of Public Policies to improve the R&D and innovation in the Brazilian Chemical Industry.

Constituintes químicos de Galianthe brasiliensis (RUBIACEAE)

This paper describes the chemical constituents isolated from aerial parts of the plant Galianthe brasiliensis. From a methanol extract, the iridoid glycosides asperuloside, deacetylasperuloside, mixture of Z- and E-6-O-p-coumaroylscandoside methyl ester, the triterpene ursolic acid and the steroids stigmasterol, campesterol, beta-sitosterol and 3-O-beta-glycopiranosyl sitosterol were isolated. The structures of the natural products were identified on the basis of spectral data, including 2D NMR experiments. The antiproliferative properties of the crude methanolic extract were investigated against a series of nine human cancer cell lines.

Determinação de resíduos de cloranfenicol em amostras de leite e mel industrializados utilizando a técnica de espectrometria de massas em "tandem" (CLAE-EM/EM)

The present work shows a method for the determination of chloramphenicol (CAP) antibiotic in milk, powder milk and honey. The solid phase extraction and liquid-liquid extraction were applied as a clean-up and pre-concentration strategies followed by LC-ESI/MS/MS analysis. The recovery was studied for different fortification levels from 0.05 to 1.00 µg L-1 in milk, showing values between 91 101% and RSD bellow 8.0%, while honey was spiked with a concentration of 0.20 µg kg-1 yelding a mean recovery of 83% and RSD of 6.5%. The quantification transition 321>152 showed a LOD of 0.52 ng kg-1 and LOQ of 1.85 ng kg-1.

Desempenho físico-químico de metais e estruturas de concreto de redes de distribuição de energia: estudo de caso na região de Manaus

The influence of natural aging furthered by atmospheric corrosion of parts of electric transformers and materials, as well as of concrete poles and cross arms containing corrosion inhibitors was evaluated in Manaus. Results for painted materials, it could showed that loss of specular gloss was more intensive in aliphatic polyurethane points than in acrylic polyurethane ones. No corrosion was observed for metal and concrete samples until 400 days of natural aging. Corrosion in steel reinforcement was noticed in some poles, arising from manufacturing faults, such as low cement content, water/cement ratio, thin concrete cover thickness, etc. The performance of corrosion inhibitors was assessed by many techniques after natural and accelerated aging in a 3.5% saline aqueous solution. The results show the need for better chemical component selection and its concentration in the concrete mixture.

Influência de desproteinizantes ácidos na quantificação da glutationa reduzida eritrocitária por CLAE-UV

Large differences in reduced glutathione (GSH) levels have been found in different investigations, also in healthy people. GSH oxidation in vitro has been associated with sample acidification in the presence of oxihemoglobin. In this work, the influence of different acids on GSH determination utilizing HPLC with UV detection was evaluated. The results showed that metaphosphoric acid and sulfosalicylic acid were inadequate for analysis, because metaphosphoric acid showed to be inefficient for deproteinization and with sulfosalicylic acid loss of GSH was observed. Trichloroacetic acid did not effect GSH quantification, since the deproteinized form was immediately derivatized with 5, 5´-dithio-bis (2-nitrobenzoic) acid. Methods with TCA deproteinization presented linear results from 0.5 to 3.0 mM. The correlation coefficient between aqueous curves and GSH spiked RBC exceeded 0.99. Precision calculations showed CV lower than 10% and bias within ± 10% for concentrations of 0.5; 1.5 and 3.0 mM GSH. The recovery was higher than 94%. Moreover, GSH blood concentrations were independent of hemoglobin concentrations.

Desenvolvimento e validação de metodologia analítica para determinação de itraconazol em produtos farmacêuticos por CLAE

Itraconazole is a synthetic antifungal drug administered orally with a broad spectrum of activity against mycotic infections. The present work consists of the development and validation of analytical methodology for evaluation of itraconazole in pharmaceutical products by high performance liquid chromatography. The separation was made using the reversed-phase column LC-18, acetonitrile/diethylamine 0.05% v/v, 60:40 v/v, pH 8.0 as mobile phase, methanol as solvent and detection and quantification at 254 nm. The results here obtained show that the analytical methodology is accurate, reproducible, robust and linear over the concentration range 8.0-12.0 µg/mL of itraconazole. The method was applied to pharmaceutical capsules containg itraconazole pellets and showed to be efficient, yielding good results.

Desenvolvimento de método analítico por CLAE em comprimidos de Benznidazol para a Doença de Chagas

The analytical method of high performance liquid chromatography (HPLC) for the assay of benznidazole in tablets was developed and validated following the requirements of regulatory agencies. The method used as mobile phase acetonitrile:wather 1:1, a C18 column of 12.5 cm length x 4 mm id, 5 mm particles and lambda=316 nm. The statistical analysis of the results demonstrated that the method satisfies all parameters so as to be considered a safe and efficient analytical alternative of low cost for laboratory routine.

Avaliação da estabilidade do marcador plasmático do estresse oxidativo: malondialdeído

Malondialdehyde (MDA) is one of the lipid peroxidation products widely used as indicator of cellular injury. However, the short-term and the long-term stability of this biomarker remain unclear. The objective of this work was to evaluate the stability of plasmatic MDA at -20 ºC, utilizing thiobarbituric acid (TBA) as derivative in spectrophotometric and chromatographic analysis. The results showed that MDA was stable for 24 h after blood collection, was not stable when stored after alkaline hydrolysis, remained stable for 30 days after TBA derivatization and was stable for 3 days when stored after n-butanol extraction, all at -20 ºC.

Validação de métodos cromatográficos por clae para análise das vitaminas B1, B2, B6 e niacina naturalmente presentes em farinha de cereais

Complex B vitamins are present in some cereal foods and the ingestion of enriched products contributes to the recommended dietary intake of these micronutrients. To adapt the label of some products, it is necessary to develop and validate the analytical methods. These methods must be reliable and with enough sensitivity to analyze complex B vitamins naturally present in food at low concentration. The purpose of this work is to evaluate, with validated methods, the content of vitamins B1, B2, B6 and niacin in five cereal flours used in food industry (oat, rice, barley, corn and wheat).

Ácidos ciclopentênicos do óleo da sapucainha (Carpotroche brasiliensis Endl, Flacourtiaceae): o primeiro antileprótico usado no Brasil

The chaoolmugra oil is one of the oldest medicines used for leprosy until the development of sulfas. In Brazil, it is known as sapucainha oil that is obtained from Carpotroche brasilienesis seeds (Flacourtiaceae). Chemical and medicinal studies of sapucainha oil were introduced in Brazil by Peckolt, Cole and Cardoso which showed that major ciclopentenyl fatty acids as chaulmoogric, hydnocarpic and gorlic were responsible for its bactericidal activity. In this work, a method for quantification of sapucainha oil acidic fraction by HRGC was established using methyl n-heptadecanoate as internal standard. The oil chemical stability was investigated by the use of GC-MS, IR, ¹H and 13C NMR and showed that the main degradation products belong to the cyclopentenyl moiety oxidation.

Estudo químico e biológico de Tephrosia toxicaria Pers.

The ethanol extracts from leaves, stems, pods and roots were assayed against the 3rd instar Aedes aegypti larvae and the highest activity was observed in the roots extracts (LC50 47.86 ppm). This extract was submitted to partition with hexane, chloroform, ethyl acetate and methanol. The respective fractions were bioassayed and the best larvicidal activities were identified in the hexane (LC50 23.99 ppm) and chloroform (LC50 13.80 ppm) fractions. Antioxidant activity (DDPH method) was observed in the ethanol extract (IC50 276 µg/mL) from roots of T. toxicaria. Fractions from this extract were also tested and the highest antioxidant activity (IC50 89 µg/mL) was found in the methanol fraction. The flavonoids iso-obovatin (1), obovatin (2), 6a,12a-dehydro-β-toxicarol (3), 6a,12a-dehydro-α-toxicarol (4) and α-toxicarol (5) were isolated and bioassayed against A. aegypti. The flavonoid 5 showed the best larvicidal activity (LC50 24.55 ppm). The antioxidant activity of 2 was investigated and showed IC50 3.370 µg/mL. The antioxidant and larvicidal activities of Tephrosia toxicaria are reported for the first time.

Biodegradação de tolueno e óleo de pescado em solos impactados utilizando surfactantes químico e biológico

The process of biodegradation of soils contaminated by animal (raw fish oil) and mineral (toluene) origin compounds was studied, verifying the influence of adding biosurfactants and chemical surfactants and nutrients in the media. The highest removal rate of fish oil was 59.47% obtained in the experiments containing biosurfactant and biostimulate in 90 days process. The highest removal rate of toluene was achieved in 14 days for experiments containing biosurfactant, chemical spreading and biosurfactant with biostimulation, showing great influence of evaporation on the process. The use of surfactants has shown to increase the contaminant bioavailability due to its higher degradation rate.

Desenvolvimento e validação de metodologia analítica por CLAE-IR para determinação de artemisinina em Artemisia annua L

The aim of this work was to develop and validate an analytical methodology for determination of artemisinin used as antimalaric. The method was based on high performace liquid chromatography, using a CN column with mobile phase composed of methanol : H2O 50:50 (V/V). The results showed that the method presented linearity from 50 to 1500 µg/mL. It was considered selective, accurate, precise according to the specific resolution from ANVISA, the Brazilian regulatory agency.

Desempenho físico-químico e mecânico de concreto de cimento Portland com borracha de estireno-butadieno reciclada de pneus

Physicochemical and mechanical techniques were carried out to characterize three concrete tyre-rubber waste dosages such as 5, 10 and 15%, w/w. The elastomeric material was identified as styrene-butadiene rubber (SBR). It was observed that the growing SBR content in the mixture decreased the concrete performance. The best results were presented by 5% w/w tyre-rubber waste concrete sample. This composition was tested at Mourão hydroelectric powerplant spillway as repairing material.

Determinação de 3,4-metilenodioximetanfetamina (MDMA) em comprimidos de Ecstasy por cromatografia líquida de alta eficiência com detecção por fluorescência (CLAE-DF)

This paper describes the development and validation of simple and selective analytical method for determination of 3.4-methylenedioxymethamphetamine (MDMA) in Ecstasy tablets, using high performance liquid chromatography with fluorescence detection. Analysis was performed in a reversed phase column (LiChrospher 100 C18, 150 x 4.6 mm, 5 µm), isocratic elution with phosphate buffer 25 mmol/L pH 3.0 and acetonitrile (95:5, v/v). The method presents adequate linearity, selectivity, precision and accuracy. MDMA concentration in analyzed tablets showed a remarkable variability (from 8.5 to 59.5 mg/tablet) although the tablet weights were uniform, indicating poor manufacturing control thus imposing additional health risks to the users.