Terbinafine: optimization of a LC method for quantitative analysis in pharmaceutical formulations and its application for a tablet dissolution test

A simple liquid chromatographic method was optimized for the quantitative determination of terbinafine in pharmaceutical hydroalcoholic solutions and tablets, and was also employed for a tablet dissolution test. The analysis was carried out using a RP-C18 (250 mm × 4.6 mm, 5 μm) Vertical® column, UV-Vis detection at 254 nm, and a methanol-water (95:5, v/v) mobile phase at a flow-rate of 1.2 mL min-1. Method validation investigated parameters such as linearity, precision, accuracy, robustness and specificity, which gave results within the acceptable range. The tablets dissolution was quite fast: 80% of the drug was dissolved within 15 min.

Quantitative structure-retention relationships analysis of retention index of essential oils

Genetic algorithm and multiple linear regression (GA-MLR), partial least square (GA-PLS), kernel PLS (GA-KPLS) and Levenberg-Marquardt artificial neural network (L-M ANN) techniques were used to investigate the correlation between retention index (RI) and descriptors for 116 diverse compounds in essential oils of six Stachys species. The correlation coefficient LGO-CV (Q²) between experimental and predicted RI for test set by GA-MLR, GA-PLS, GA-KPLS and L-M ANN was 0.886, 0.912, 0.937 and 0.964, respectively. This is the first research on the QSRR of the essential oil compounds against the RI using the GA-KPLS and L-M ANN.

Gemifloxacin mesylate: UV spectrophotometric method for quantitative determination using experimental design for robustness

This study describes the validation of UV spectrophotometric method for quantitative determination of gemifloxacin mesylate (GFM) in tablets using methanol as solvent. The method was specific, linear, precise, exact and robust at 272 and 343 nm. The results confirmed that the method in both wavelengths is valid and useful to the routine quality control of GFM in coated tablets. The validate method was compared to liquid chromatography (HPLC), microbiological assay and visible (VIS) spectrophotometry, which were previously developed and validated to the same drug. There was not significative difference between the methods for GFM quantitation.

A quantitative validated method using liquid chromatography and chemometric analysis for evaluation of raw material oF Maytenus ilicifolia (Schrad.) Planch., Celastraceae

The hydroalcoholic extracts prepared from standard leaves of Maytenus ilicifolia and commercial samples of espinheira-santa were evaluated qualitatively (fingerprinting) and quantitatively. In this paper, fingerprinting chromatogram coupled with Principal Component Analysis (PCA) is described for the metabolomic analysis of standard and commercial espinheira-santa samples. The epicatechin standard was used as an external standard for the development and validation of a quantitative method for the analysis in herbal medicines using a photo diode array detector. This method has been applied for quantification of epicatechin in commercialized herbal medicines sold as espinheira-santa in Brazil and in the standard sample of M. ilicifolia.

Isolation and quantitative HPLC-PDA analysis of lupeol in phytopharmaceutical intermediate products from Vernonanthura ferruginea (Less.) H. Rob.

Prior to obtain a standardized dried extract from V. ferruginea, lupeol was first time isolated from leaves and used as chemical maker. An analytical method using HPLC-PDA for lupeol determination in V. ferruginea intermediate products was developed using a C8 reverse-phase column, acetonitrile-acetic acid (99.99:0.01, v/v) as mobile phase at 0.8 mL min-1, oven temperature at 23-25 ºC, sample injection volume at 30 µL and detection at 210 nm. The method presented linearity from 10 to 160 µg mL-1, accuracy, precision, robustness and suitable sensitivity proving to be a useful tool to the obtainment process of lupeol standardized dried extracts of V. ferruginea.

Quantitative analysis of two important epidemiological features of the common bean: Phaeoisariopsis griseola pathosystem

This work quantifies two important epidemiological features of the bean (Phaseolus vulgaris)/Phaeoisariopsis griseola pathosystem. The first is the effect of the number of nights of leaf wetness on infection efficiency. Infection efficiency was below 10% when inoculated leaflets were exposed to less than two nights of leaf wetness. Optimum infection efficiencies were obtained after three to four nights of leaf wetness, at about 50%. Further nights of leaf wetness did not increase the infection efficiency. The second feature quantified is the relative rate of leaflet defoliation for varying levels of angular leaf spot severity. It increased with disease severity according to a logarithm-like curve, and a relative rate of 0.23 day-1 was estimated for a severity of 18%. The implications of these results on the disease epidemiology are discussed.

Flow injection visible diffuse reflectance quantitative analysis of total sulfur in biodiesel, in plant leaves and in natural waters

Flow injection (FI) methodology, using diffuse reflectance in the visible region of the spectrum, for the analysis of total sulfur in the form of sulfate, precipitated in the form of barium sulfate, is presented. The method was applied to biodiesel, to plant leaves and to natural waters analysis. The analytical signal (S) correlates linearly with sulfate concentration (C) between 20 and 120 ppm, through the equation S=-1.138+0.0934 C (r = 0.9993). The experimentally observed limit of detection is about 10 ppm. The mean R.S.D. is about 3.0 %. Real samples containing sulfate were analyzed and the results obtained by the FI and by the reference batch turbidimetric method using the statistical Student's t-test and F-test were compared.

Spot-test identification and rapid quantitative sequential analysis of dipyrone

A qualitative spot-test and tandem quantitative analysis of dipyrone in the bulk drug and in pharmaceutical preparations is proposed. The formation of a reddish-violet color indicates a positive result. In sequence a quantitative procedure can be performed in the same flask. The quantitative results obtained were statistically compared with those obtained with the method indicated by the Brazilian Pharmacopoeia, using the Student's t and the F tests. Considering the concentration in a 100 µL aliquot, the qualitative visual limit of detection is about 5×10-6 g; instrumental LOD ≅ 1.4×10-4 mol L-1 ; LOQ ≅ 4.5×10-4 mol L-1.

Quantitative control of Lettuce mosaic virus fitness and host defence inhibition by P1-HCPro

Two Lettuce mosaic virus isolates capable of overcoming the resistance afforded by the resistance gene mo1² in lettuce, LMV-AF199 from Brazil, and LMV-E, an European isolate, were evaluated for the rapidity and severity of symptoms induced on the lettuce variety Salinas 88 (mo1²). The mosaic symptoms on Salinas 88 plants inoculated with LMV-AF199 appeared 7 days post-inoculation (dpi) and 15 dpi for LMV-E. The symptoms induced by LMV-AF199 in this cultivar were also more severe than those induced by LMV-E. In order to identify the region of the viral genome responsible for this phenotype, recombinant viruses were constructed between these isolates and the phenotype of each recombinant was analysed. The region encoding proteins P1 and HcPro from LMV-AF199 was associated with the increased virulence in Salinas 88.

Canopy openness and lai estimates in two seasonally deciduous forests on limestone outcrops in central Brazil using hemispherical photographs

Patches of seasonally dry tropical forests occur on limestone outcrops in Central Brazil surrounded by the dominant savanna vegetation. They contain valuable timber species but are threatened by farming and mining activities. The objective of this study was to describe canopy opening and light relations in two seasonally deciduous dry forests on slopes and limestone outcrops, in the Paranã valley at the northeastern region of the Goiás state, Brazil. The studied forests were in the Fazenda Sabonete in Iaciara-Go and Fazenda Forquilha in Guarani-GO. Woody plants were sampled in 25 (20 x 20 m) plots in each forest. In the Sabonete forest 40 species, 705 ind./ha-1 with a basal area of 15.78 m²/ha-1 were found, while in Forquilha there were 55 species, 956 ind./ha-1 with a basal area of 24.76 m²/ha-1. Using hemispherical photographic techniques, 25 black and white photographs were taken at each site, during the dry season, totaling 50 photographs. These were taken at the beginning of each vegetation-sampling plot. The photographs were scanned in grey tones and saved as 'Bitmap'. The canopy opening and leaf area index (LAI) were calculated using the software Winphot. The mean canopy opening was 54.0% (±9.36) for Fazenda Sabonete and 64.6% (±11.8) in Fazenda Forquilha, with both sites presenting significant differences in the opening estimates (P < 0.05). Their floristic richness and structure also differed with the more open canopy forest, Forquilha, being richer and denser, suggesting the need for further studies on species-environment relationships in these forests.

Relationships and estimates of longitudinal growth stress in Eucalyptus dunnii at different ages

The objective of this study was to obtain estimates of longitudinal growth stresses in standing trees of the Eucalyptus dunnii Maiden at eight, thirteen, fifteen and nineteen years of age and to determine their relationships with wood characteristics. The longitudinal growth stresses were indirectly measured by the "CIRAD-Forêt" method and estimated from both the dynamic modulus of elasticity and the modulus of elasticity in tension parallel to the grain. The longitudinal residual strain (LRS) and the estimates of the longitudinal growth stresses tended to increase with the age of the material. The LRS correlated positively and significantly with all the growth stresses estimates. The largestes magnitudes were at 13, 15 and 19 years of age. The basic density presented high, positive and significant correlations with the dynamic modulus of elasticity, estimated in the longitudinal direction, for wood saturated and at 12% moisture content, for all the ages assessed. All the growth stresses estimates presented high, positive and significant correlations between themselves.

ABOVEGROUND AND BELOWGROUND BIOMASS AND CARBON ESTIMATES FOR CLONAL EUCALYPTUS TREES IN SOUTHEAST BRAZIL

Eucalyptus plantations represent a short term and cost efficient alternative for sequestrating carbon dioxide from the atmosphere. Despite the known potential of forest plantations of fast growing species to store carbon in the biomass, there are relatively few studies including precise estimates of the amount of carbon in these plantations. In this study it was determined the carbon content in the stems, branches, leaves and roots of a clonal Eucalyptus grandis plantation in the Southeast of Brazil. We developed allometric equations to estimate the total amount of carbon and total biomass, and produced an estimate of the carbon stock in the stand level. Altogether, 23 sample trees were selected for aboveground biomass assessment. The roots of 9 of the 23 sampled trees were partially excavated to assess the belowground biomass at a singletree level. Two models with DBH, H and DBH2H were tested. The average relative share of carbon content in the stem, branch, leaf and root compartments was 44.6%, 43.0%, 46.1% and 37.8%, respectively, which is smaller than the generic value commonly used (50%). The best-fit allometric equations to estimate the total amount of carbon and total biomass had DBH2H as independent variable. The root-to-shoot ratio was relatively stable (C.V. = 27.5%) probably because the sub-sample was composed of clones. Total stand carbon stock in the Eucalyptus plantation was estimated to be 73.38 MgC ha-1, which is within the carbon stock range for Eucalyptus plantations.

Quali/quantitative characterization of biogas produced in batch digesters supplied with six distinct substrates

The present research was carried out at the DER/FCAV, São Paulo State University - Brazil, with the purpose of analyzing the quantity and quality of biogas produced by six types of substrates. The substrates used in the anaerobic digestion were characterized as: 1- Litter of broiler (LB); 2- Grinded broiler litter (GBL); 3- Broiler litter with wood shavings (BLWS); 4- Grinded broiler litter with wood shavings (GBLWS); 5- Broiler litter with peanut hulls (BLPH); 6- Grinded broiler litter with peanut hull (GBLPH). It was concluded from the collected data that: the (GBL) substrate showed a superior biogas accumulated production in relation to the other substrates, while the BLWS presented an inferior accumulated production; the grinded substrates showed higher quantities of accumulated biogas in relation to the non-grinded substrates, except for GBLPH, with 20.9 m³ inferior than BLPH; the period of maximum biogas production started from 45 to 60 days, declining after 120 days; at 57 days after filling up the digesters the biogas produced had levels of CH4 superior than 53%, and from 99 days all of them produced biogas with levels of CH4 superior than 70%; LB and GBL presented higher concentrations of CH4 in the biogas.

Uncertainties of the 137Cs technique for validation of soil redistribution modelling in a semiarid meso-scale watershed

Scarcity of long-term series of sediment-related variables has led watershed managers to apply mathematical models to simulate sediment fluxes. Due to the high efforts for installation and maintenance of sedimentological gauges, tracers have been pointed out as an alternative to validate soil redistribution modelling. In this study, the 137Cs technique was used to assess the WASA-SED model performance at the Benguê watershed (933 km²), in the Brazilian semiarid. Qualitatively, good agreement was found among the 137Cs technique and the WASA-SED model results. Nonetheless, quantitatively great differences, up to two orders of magnitude, were found between the two methods. Among the uncertainties inherent to the 137Cs technique, definition of the reference inventory seems to be a major source of imprecision. In addition, estimations of water and sediment fluxes with mathematical models usually also present high uncertainty, contributing to the quantitative differences of the soil redistribution estimates with the two methods.

Low-flow estimates in regions of extrapolation of the regionalization equations: a new concept

ABSTRACT Knowledge of natural water availability, which is characterized by low flows, is essential for planning and management of water resources. One of the most widely used hydrological techniques to determine streamflow is regionalization, but the extrapolation of regionalization equations beyond the limits of sample data is not recommended. This paper proposes a new method for reducing overestimation errors associated with the extrapolation of regionalization equations for low flows. The method is based on the use of a threshold value for the maximum specific low flow discharge estimated at the gauging sites that are used in the regionalization. When a specific low flow, which has been estimated using the regionalization equation, exceeds the threshold value, the low flow can be obtained by multiplying the drainage area by the threshold value. This restriction imposes a physical limit to the low flow, which reduces the error of overestimating flows in regions of extrapolation. A case study was done in the Urucuia river basin, in Brazil, and the results showed the regionalization equation to perform positively in reducing the risk of extrapolation.