Performance characteristics of bioassay UV-spectrophotometry and high perfomance liquid chromatographic determination of gatifloxacin in tablets

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Off line extraction of phenol from human urine sample with isoamyl alcohol and determination by HPLC

This method has been developed for extraction and determination of phenol in a urine sample by high performance liquid chromatography.After acid hydrolysis, the free phenol was extracted with isoamyl alcohol solvent, followed by back extraction with 0.5 mol.L-1 sodium hydroxide solution and analyzed by an isocratic HPLC Varian System, equipped with reverse-phase column (MicroPak-C-18). The mobile phase was acetonitrile in 0.01 mol.L-1 hydrochloric acid solution, (20:80 v/v), and at a now-rate of 1.0 mL.min-1. The chromatogram was monitored at 220 nm in room temperature. The identification was based on retention time and the quantification was performed by automatic peak-area determination, corrected for the external standards method.The recovery was higher than 99.5 % for phenol and reproducibility of method was shown to be 2.3% standard deviation and 5.6% coefficient of variance (n=20). The limit detection was 0.05 mgL(-1) and a range of 0.05 to 20.0 mgL(-1) of phenol for linearity.

High-performance liquid chromatographic separation and identification of polyphenolic compounds from the infusion of Davilla elliptica St. Hill

The isolation of polyphenolic compounds from an infusion of the Brazilian plant Davilla elliptica (Dilleniaceae), used as tea by virtue of its digestive properties, is described. An improved preparative HPLC method was used in order to isolate pure polyphenols from the complex mixture. Liquid-liquid extraction and solid-phase extraction were employed to minimise the interference of polymeric compounds and to provide an enriched fraction of the compounds of interest. The identification of the isolated compounds was performed using analytical HPLC as well as direct injection electrospray ionisation ion trap tandem mass spectrometry (ESI-IT-MS/MS). The high flavonoid content suggests that D. elliptica may be a promising source of compounds to produce natural phytomedicines. Copyright (C) 2007 John Wiley & Sons, Ltd.

Effects of the high temperature plasma immersion ion implantation (PIII) of nitrogen in AISI H13 steel

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Síntese enzimática de biosurfactante e sua aplicabilidade na indústria do petróleo

Enzymes have been widely used in biosynthesis/transformation of organic compounds in substitution the classic synthetic methods. This work is the first writing in literature of enzymatic synthesis for attainment the biossurfactants, the use glucose sucrose, ricinoleic acid e castor oil as substratum, and as biocatalyst, used immobilized lipase Thermomyces lanuginose, Rhizomucor miehei and the Candida antarctica lipase B; alkaline protease and neutral protease from Bacillus subtillis and yeast Saccharomyces cerevisiaeI. The analysis of HPLC (high performance liquid chromatography) showed that highest conversions were reached of used the alkaline protease from Bacillus subtillis. Laboratory tests, to evaluate the applicability, indicated that the produced biosurfactantes had good stability in presence of salts (NaCl) and temperature (55 e 25°C), they are effective in the reduction of the superficial tension and contac angle, but they have little foaming capacity, when compared with traditional detergents. These results suggest that the prepared surfactants have potential application as wetting agent and perforation fluid stabilizer

Rat model of depending prostaglandin renal state: Effect of ketoprofen

Introduction .The renal prostaglandins (PGs), vasodilators, preserve kidney function during increased activity of the renin-angiotensin system or renal sympathetic nerves (renal PG-dependent state [RPGD]). Ketoprofen (Ket) inhibits cyclooxygenase and, therefore, the synthesis of PGs. The aim of this study was to determine, in the rat, the action of Ket in the renal histology and function in a RPGD state (stress of anesthesia and hemorrhage). Material and Methods . Twenty male Wistar rats, anesthetized with sodium pentobarbital, were randomly divided into two groups: G1-control ( n = 10) and G2-Ket ( n = 10) submitted to arterial hemorrhage of 30% of volemia (estimated as 6% of body weight) three times (10% each 10 min), 65 min after anesthesia. G2 animals received Ket, 1.5 mg. kg -1 , venously, 5 min after anesthesia and 60 min before the first hemorrhage moment (first moment of the study [M1]). Medium arterial pressure (MAP), rectal temperature (T), and heart rate were monitored. G1 and G2 received para-aminohippurate sodium (PAH) and iothalamate sodium (IOT) solutions during the entire experimental time in order to determine clearance of PAH (effective renal plasma flow [ERPF]) and clearance of IOT (glomerular filtration rate [GFR]) without urine collection (determination of blood concentrations of PAH and IOT through the high-performance liquid chromatography), filtration fraction (FF), and renal vascular resistance (RVR). The animals were sacrificed in M3, 30 min after the third hemorrhage (M2) moment, and the kidneys and blood collected during the hemorrhage periods were utilized for histological study and determinations of hematocrit (Ht), serum creatinine (S Cr ), ERPF, GFR, FF, and RVR, respectively. Results . There were significant reductions of MAP, T, and Ht and a significant increase of S Cr . During the experiment, ERPF and GFR did not change, but ERPF was always higher in G1 than in G2. Ket did not alter FF, which increased in G1 over the duration of experiment. The Ket group had significantly higher RVR than the control group. The histology verified that both G1 and G2 were similar for tubular dilation and necrosis, but they were significantly different for tubular degeneration: G1 > G2. Conclusion . The changes observed in kidney histology probably were determined by hemorrhage and hypotension. Ket inhibited the synthesis of PGs and diminished tubular degeneration.

Aspirin increases tolerance to high temperature in seeds of Raphanus sativus L. cvar Early Scarlet Globe

The incubation of seeds of Raphanus sativus L. cvar Early Scarlet Globe with 10 mu M aspirin resulted in increase in the temperature range for germination. The analysis of percentage germination and germination rates indicated the increase in the optimum temperature from 21.4 to 26 degrees C although at 32.6 degrees C 80.8% of seeds germinated with aspirin and no germination in the control. The analysis of the kinetics of seed germination indicated that aspirin treatment resulted in germination by decreasing the enthalpy of activation of the process. The aspirin treatment also resulted in the synchronization of seed germination. on the base of our results we propose aspirin application in practice to increase the tolerance to high temperature and to synchronize seed germination at least in Raphanus sativus L. cvar early scarlet globe.

The identification of beta-thalassemia mutants in Brazilians with high Hb F levels

As hemoglobinopatias são um grupo de afecções genéticas que representam problema de saúde pública em muitos países em que sua incidência é alta, com significativa morbidade. Objetivamos identificar defeitos moleculares que pudessem explicar o perfil laboratorial obtido por eletroforese e HPLC com Hb F elevada, em um grupo de indivíduos adultos sem sinais ou sintomas de anemia. Encontramos cinco diferentes mutações que originam beta talassemia por PCR-ASO: três casos com CD 6 (-A), um CD 39, um IVS 1-5, um -87 todas de origem mediterrânea, e um IVS II-654 de origem asiática. As mutações CD 6 (-A), -87 e IVS II-654 foram descritas pela primeira vez na população brasileira.

Voltage-composition profile and synchrotron X-ray structural analysis of low and high temperature LixCoO2 host material

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Loading of praziquantel in the crystal lattice of solid lipid nanoparticles Studies by DSC and SAXS

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Monitoring pharmaceuticals photo-Fenton degradation process by using Solid Phase Extraction and liquid chromatography

The recovery of the pharmaceuticals bezafibrate and tetracycline from water was evaluated, using Solid Phase Extraction (SPE) with the aim of applying this technique to interrupt the pharmaceuticals' photodegradation by photo-Fenton process for further analysis. Sep-Pack C-18, Strata X, and Oasis HLB cartridges were evaluated. Oasis HLB showed the most satisfactory recovery and repeatability results: 98% (CV - 1%) for bezafibrate (20.0 mg L-1) and 76% (CV = 1%) for tetracycline (25.0 mg L-1). There was not a significant decrease in recovery at lower concentrations of the pharmaceuticals, and neither when present in Sewage Treatment Plant (STP) effluent matrix.

Characterization of flavonoid and naphthopyranone derivatives from Eriocaulon ligulatum using liquid chromatography tandem mass spectrometry

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Identification of triterpenes and sterols from pterogyne nitens (fabaceae-caesalpinioideae) using high-resolution gas chromatography

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

The role of matrix effects on the quantification of abscisic acid and its metabolites in the leaves of Bauhinia variegata L. using liquid chromatography combined with tandem mass spectrometry

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Organic acid profile of commercial sour cassava starch

A presença de ácidos orgânicos no polvilho azedo, além de contribuir com aspectos como sabor e aroma, tem, conforme a literatura indica, correlação com a propriedade de expansão, que é um fator determinante no uso alimentício. Amostras de polvilho azedo foram coletadas nas Regiões Sul e Sudeste diretamente nas empresas ou no comércio. Foram preparadas para análise em cromatografia líquida de alta eficiência (CLAE), sendo que o cromatógrafo estava equipado com coluna Biorad Aminex HPX-87H para análise de ácidos orgânicos e detector refratométrico. As condições de análise envolveram o emprego da fase móvel ácido sulfúrico 0,005M, fluxo de 0,6 ml/min e temperatura da coluna de 60oC. Os ácidos quantificados foram lático (0,036 a 0,813 g/100g), acético (0 a 0,068 g/100g), propiônico (0 a 0,013 g/100g) e butírico (0 a 0,057 g/100g), presentes na fermentação natural. Os resultados revelaram grande variação entre as amostras, com diferenças mesmo dentro das Regiões. Algumas amostras apresentaram quantidades elevadas de ácidos, especialmente do ácido lático, mas nestas amostras os ácidos propiônico e butírico não foram detectados. A ausência do ácido butírico não era esperada, uma vez que esse ácido está diretamente relacionado com o aroma característico do polvilho azedo. O fato pode sugerir que a obtenção de algumas das amostras estudadas pode ter ocorrido sem o processo fermentativo natural.