Preparation and electrochemical characterization of Pt nanoparticles dispersed on niobium oxide

Electrodes consisting of Pt nanoparticles dispersed on thin films of niobium oxide were prepared onto titanium substrates by a sol-gel method. The physical characterization of these electrodes was carried out by X-ray diffraction, scanning electron microscopy and energy dispersive X-ray analysis. The mean size of the Pt particles was found to be 10.7 nm. The general aspects of the electrochemical behavior were studied by cyclic voltammetry in 1 mol L-1 HClO4 aqueous solution. The response of these electrodes in relation to the oxidation of formaldehyde and methanol in acidic media was also studied.

A direct potentiometric titration study of the dissociation of humic acid with selectively blocked functional groups

A direct potentiometric titration method was applied to commercial and soil humic acids in order to determine their carboxyl and phenol group concentrations and apparent and intrinsic pK. In that context, acid-base properties of humic acids are interpreted by selective blocking of carboxylic and phenolic groups by esterification and acetylation. Differences in underivatized and derivatized HA's acid-base properties are ascribed to carboxyl and phenol groups influence on total humic acidity. Potentiometric data were treated with the modified Henderson-Hasselbalch equation. Infra red results, the acidic group contents and the average values of apparent and intrinsic pK for underivatized and derivatized HAs confirmed the selectivity of esterification derivatization method. After blocking of the functional groups, the values of acidic group contents decreased, while the value of apparent pK increased after derivatization. Phenol groups cannot be specifically identified by the acetylation method, due to low selectivity of the acetylation method.

Sensitive spectrophotometric determination of lansoprazole in pharmaceuticals using ceric ammonium sulphate based on redox and complex formation reactions

Two simple sensitive and cost-effective spectrophotometric methods are described for the determination of lansoprazole (LPZ) in bulk drug and in capsules using ceric ammonium sulphate (CAS), iron (II), orthophenanthroline and thiocyanate as reagents. In both methods, an acidic solution of lansoprazole is treated with a measured excess of CAS followed by the determination of unreacted oxidant by two procedures involving different reaction schemes. The first method involves the reduction of residual oxidant by a known amount of iron(II), and the unreacted iron(II) is complexed with orthophenanthroline at a raised pH, and the absorbance of the resulting complex measured at 510 nm (method A). In the second method, the unreacted CAS is reduced by excess of iron (II), and the resulting iron (III) is complexed with thiocyanate in the acid medium and the absorbance of the complex measured at 470 nm (method B). In both methods, the amount CAS reacted corresponds to the amount of LPZ. In method A, the absorbance is found to increase linearly with the concentration of LPZ where as in method B a linear decrease in absorbance occurs. The systems obey Beer's law for 2.5-30 and 2.5-25 µg mL-1 for method A and method B, respectively, and the corresponding molar absorptivity values are 8.1×10³ and 1.5×10(4) L mol-1cm-1 . The methods were successfully applied to the determination of LPZ in capsules and the results tallied well with the label claim. No interference was observed from the concomitant substances normally added to capsules.

Spectrophotometric determination of mosapride in pure and pharmaceutical preparations

Two simple and sensitive spectrophotometric methods (M1 and M2) for the determination of mosapride in pure and in pharmaceutical preparations are described. These methods are based on the interaction of diazotized mosapride (MSP) couples with chromotropic acid (CTA) [M1] in alkaline medium and diphenylamine (DPA) [M2] in acidic medium. The resulting azo-dyes exhibit maximum absorption at 560 nm and at 540 nm for methods M1 and M2, respectively. All variables were studied in order to optimize the reaction conditions. No interferences were observed from excipients, and the validity of the each method was tested against reference method.

Simple and sensitive spectrophotometric methods for the determination of acebutolol hydrochloride in bulk sample and pharmaceutical preparations

A direct, extraction-free spectrophotometric method has been developed for the determination of acebutolol hydrochloride (ABH) in pharmaceutical preparations. The method is based on ion-pair complex formation between the drug and two acidic dyes (sulphonaphthalein) namely bromocresol green (BCG) and bromothymol blue (BTB). Conformity to Beer's law enabled the assay of the drug in the range of 0.5-13.8 µg mL-1 with BCG and 1.8-15.9 µg mL-1 with BTB. Compared with a reference method, the results obtained were of equal accuracy and precision. In addition, these methods were also found to be specific for the analysis of acebutolol hydrochloride in the presence of excipients, which are co-formulated in the drug.

A simple method for the spectrophotometric determination of cephalosporins in pharmaceuticals using variamine blue

A simple spectrophotometric method for the determination of cefotaxime, ceftriaxone, cefadroxil and cephalexin with variamine blue is presented. The determination is based on the hydrolysis of β-lactam ring of cephalosporins with sodium hydroxide which subsequently reacts with iodate to liberate iodine in acidic medium. The liberated iodine oxidizes variamine blue to violet colored species of maximum absorption at 556 nm. The absorbance is measured within the pH range of 4.0-4.2. Beer's law is obeyed in the range of 0.5-5.8 µg mL-1, 0.2-7.0 µg mL-1, 0.2-5.0 µg mL-1 and 0.5-8.5 µg mL-1 for cefotaxime, ceftriaxone, cefadroxil and cephalexin respectively. The analytical parameters were optimized and the method is successfully applied for the determination of cefotaxime, ceftriaxone, cefadroxil and cephalexin in pharmaceuticals.

Highly sensitive spectrophotometric methods for the determination of olanzapine

Highly sensitive and selective spectrophotometric methods (A and B) were developed for the determination of micro amounts of olanzapine (OLZ). Method A (direct method) is based on the oxidation of olanzapine with a known excess of iodine monochloride (ICl) in an acidic medium. Under the same condition, thymol blue was iodinated by unreacted ICl, and the absorbance of uniodinated thymol blue was measured at 536 nm. The decrease in ICl concentration is a measure of drug concentration. In method B (indirect method), oxidation of OLZ by a known excess of Ce(IV) in sulfuric acid medium followed by the reaction of unreacted Ce(IV) with leuco crystal violet (LCV) to crystal violet (CV), which is measured in an acetate buffer medium ( pH 4.9) at 580 nm. These methods obey the Beer's law in the concentration range of 0.2-1.6 µg mL-1 (method A) and 0.1-1.4 µg mL-1 (method B). The developed procedures have been successfully applied to the determination of OLZ in pure and in dosage forms. The results exhibit no interference from the presence of excipients. The reliability of the methods was established by parallel determination of OLZ against the reference method.

Titrimetric assay of lisinopril in aqueous and non-aqueous media

Four simple titrimetric procedures are described for the determination of lisinopril (LNP) in bulk and in pharmaceuticals based on the neutralization of basic-amino and acidic carboxylic acid groups present in LNP. Method A is based on the neutralization of basic amino groups using perchloric acid as titrant in anhydrous acetic acid medium. Method B, method C and method D are based on neutralization of carboxylic acid group using NaOH, sodium methoxide and methanolic KOH, as titrants, respectively. Method A is applicable over 2.0-20.0 mg range and the calculations are based in the molar ratio of 1:2 (LNP:HClO4). Method B, method C and method D are applicable over 2.0-20.0 mg, 1.0-10.0 mg and 5.0-15.0 mg range, respectively, and their respective molar ratios are 1:1 (LNP:NaOH), 1:2 (LNP:CH3ONa) and 1:1 (LNP:KOH). Intraday and inter day accuracy and precision of the methods were evaluated and the results showed intra- and inter-day precision less than 2.7% (RSD), and accuracy of < 2.5 % (RE). The developed methods were applied to determine LNP in tablets and the results were validated statistically by comparing the results with those of the reference method by applying the Student's t-test and F-test. The accuracy was further ascertained by recovery studies via standard addition technique. No interferences from common tablet exipients was observed.

Conservative nutrient use by big-leaf mahogany (Swietenia macrophylla king) planted under contrasting environmental conditions

We analyzed the nutritional composition and isotope ratios (C and N) of big-leaf mahogany (Swietenia macrophylla King) leaves in plantations established on contrasting soils and climates in Central America (State of Quintana Roo, Yucatán, México) and South America (State of Pará, Brazil). The objective was to determine the adaptability of this species to large differences in nutrient availability and rainfall regimes. Nutrient concentrations of leaves and soils were determined spectrophotometrically, and isotope ratios were measured using mass spectrometric techniques.In Pará soils were sandier, and acidic, receiving above 2000 mm of rain, whereas in Quintana Roo soils were predominantly clayey, with neutral to alkaline pH due to the underlying calcareous substrate, with about 1300 mm of rain. Leaf area/weight ratio was similar for both sites, but leaves from Quintana Roo were significantly smaller. Average N and K concentrations of adult leaves were similar, whereas Ca concentration was only slightly lower in Pará in spite of large differences in Ca availability. Leaves from this site had slightly higher P and lower Al concentrations. Differences in water use efficiency as measured by the natural abundance of 13C were negligible, the main effect of lower rainfall in Quintana Roo seemed to be a reduction in leaf area. The N isotope signature (δ15N) was more positive in Pará than in Quintana Roo, suggesting higher denitrification rates in the former. Results reveal a calciotrophic behavior and a remarkable capacity of mahogany to compensate for large differences in soil texture and nutrient availability.

Standardization of metachromatic staining method of myofibrillar ATPase activity of myosin to skeletal striated muscle of mules and donkeys

This study aims at standardizing the pre-incubation and incubation pH and temperature used in the metachromatic staining method of myofibrillar ATPase activity of myosin (mATPase) used for asses and mules. Twenty four donkeys and 10 mules, seven females and three males, were used in the study. From each animal, fragments from the Gluteus medius muscle were collected and percutaneous muscle biopsy was performed using a 6.0-mm Bergström-type needle. In addition to the metachromatic staining method of mATPase, the technique of nicotinamide adenine dinucleotide tetrazolium reductase (NADH-TR) was also performed to confirm the histochemical data. The histochemical result of mATPase for acidic pre-incubation (pH=4.50) and alkaline incubation (pH=10.50), at a temperature of 37ºC, yielded the best differentiation of fibers stained with toluidine blue. Muscle fibers were identified according to the following colors: type I (oxidative, light blue), type IIA (oxidative-glycolytic, intermediate blue) and type IIX (glycolytic, dark blue). There are no reports in the literature regarding the characterization and distribution of different types of muscle fibers used by donkeys and mules when performing traction work, cargo transportation, endurance sports (horseback riding) and marching competitions. Therefore, this study is the first report on the standardization of the mATPase technique for donkeys and mules.

Influence of environmental factors on seed germination and seedling emergence of yellow sweet clover (Melilotus officinalis)

Laboratory and greenhouse experiments were conducted to determine the effects of drought and salinity stress, temperature, pH and planting depth on yellow sweet clover (Melilotus officinalis) germination and emergence. Base, optimum and ceiling germination temperatures were estimated as 0, 18.47 and 34.60 ºC, respectively. Seed germination was sensitive to drought stress and completely inhibited at a potential of -1 MPa, but it was tolerant to salinity. Salinity stress up to 90 mM had no effect over the M. officinalis seed germination, but the germination decreased by increasing the salt concentration. The drought and salinity required for 50% inhibition of maximum germination were 207 mM and -0.49 MPa, respectively. High percentage of seed germination (>92%) was observed at pH = 5-6 and decreased to 80% at acidic medium (pH 4) and to 42% at alkaline medium (pH 9) pH. Maximum seedling emergence occurred when the seeds were placed at 2 cm depth and decreased when increasing the depth of planting; no seed emerged from depths of 10 cm.

Influence of seed size and ecological factors on the germination and emergence of field bindweed (Convolvulus arvensis)

An understanding of seed germination ecology of weeds can assist in predicting their potential distribution and developing effective management strategies. Influence of environmental factors and seed size on germination and seedling emergence of Convolvulus arvensis (field bindweed) was studied in laboratory and greenhouse conditions. Germination occurred over a wide range of constant temperatures, between 15 and 40 ºC, with optimum germination between 20 and 25 ºC. Time to start germination, time to 50% germination and mean germination time increased while germination percentage and germination index decreased with an increase in temperature from 20 ºC, salinity and osmotic stress. However, germination was tolerant to low salt (25 mM) or osmotic stress (0.2 MPa), but as salinity and osmotic stress increased, germination percentage and germination index decreased. Seeds of C. arvensis placed at soil surface showed maximum emergence and decreased as seeding depth increased. Seeds of C. arvensis germinated over a wide range of pH (4 to 9) but optimum germination occurred at pH 6 to 8. Under highly alkaline and acidic pH, time to start germination, time to 50% germination and mean germination time increased while germination percentage and germination index decreased. Increase in field capacity caused decreased time to start germination, time to 50% germination and mean germination time but increased germination percentage and germination index. Bigger seeds had low time to start germination, time to 50% germination and mean germination time but high germination percentage and germination index. Smaller seeds were more sensitive to environmental factors as compared to larger or medium seeds. It can be concluded that except for pH, all environmental factors and seed sizes adversely affect C. arvensis as regards seed germination or emergence and germination or emergence traits, and larger seeds result in improved stand establishment and faster germination than small seeds, regardless of moisture stress or deeper seeding depth.

Seed germination and seedling emergence of velvetleaf (Abutilon theophrasti) and Barnyardgrass (Echinochloa crus-galli)

Abutilon theophrasti and Barnyardgrass (Echinochloa crus-galli) are major weeds that affect cropping systems worldwide. Laboratory and greenhouse studies were conducted to determine the effects of temperature, pH, water and salinity stress, and planting depth on seed germination and seedling emergence of Velvetleaf and Barnyardgrass. For Velvetleaf, the base, optimum and ceiling germination temperatures were estimated as 5, 35 and 48 ºC, respectively. Seed germination was sensitive to drought stress and completely inhibited by a potential of -0.6 MPa, but it was tolerant to salinity. Salinity stress up to 45 mM had no effect on the germination of Velvetleaf, but germination decreased with increasing salt concentration. Drought and salinity levels for 50% inhibition of maximum germination were -0.3 MPa and 110 mM, respectively. Seed germination of Velvetleaf was tolerant to a wide range of pH levels. For Barnyardgrass, the base, optimum and ceiling germination temperatures were estimated as 5, 38 and 45 ºC, respectively. Seed germination was tolerant to drought stress and completely inhibited by a potential of -1.0 MPa. Salinity stress up to 250 mM had no effect on seed germination. Drought and salinity levels for 50% inhibition of maximum germination were -0.5 MPa and 307 mM, respectively. A high percentage of seed germination was observed at pH=5 and decreased to 61.5% at acidic medium (pH 4) and to 11% at alkaline medium (pH 9). Maximum seedling emergence of Velvetleaf and Barnyardgrass occurred when the seeds were placed on the surface of the soil or at a depth of 1 cm.

Atlantic Forest succession over calcareous soil, Parque Estadual Turístico do Alto Ribeira - PETAR, SP

The forest succession after abandonment of slash-and-burn agriculture over calcareous soil in Brazilian Atlantic Forest was assessed. This is one of the world's most threatened Biome, with only 8% remaining. The study area is located over calcareous soil inside the Alto Ribeira Touristic State Park (PETAR), southeast Brazil. The phytossociological survey showed a successional pattern dominated by species of Leguminosae, especially Piptadenia gonoacantha (Mart.) J.F. Macbr. This species occurs in calcareous soils as a substitute of Tibouchina pulchra (Cham.) Cogn. (Melastomataceae) that is the most usual dominant tree species in early succession over acidic soil, which is the most common situation in this Biome. These results are important for a better understanding of Neotropical forest biodiversity and characterize a unique genetic bank in this highly endangered Biome. They are also decisive to support actions regarding rehabilitation of degraded lands and a potential tool for Neotropical forest sustainable management, both inside and around the conservation unit.

Floristics, structure and soil of insular vegetation in four quartzite-sandstone outcrops of "Chapada Diamantina", Northeast Brazil

Soil islands on rocky surfaces often harbor aggregated vegetation that consists of insular plant communities. These islands are typical of the rocky outcrops and in various parts of Brazil form the so-called "campos rupestres" vegetation. Four of such sites have been selected in the state of Bahia, Northeast Brazil, for this comparative study on floristics and vegetation structure: three areas situated inside the "Parque Nacional da Chapada Diamantina" (Guiné, Fumaça and "Gerais da Fumaça") and one is at the border of the Environmental Protection Area of "Marimbus-Iraquara" ("Mãe Inácia"). All occurring vegetation islands were studied in four random plots of 10 × 10 m per site. Soil was often shallow, sandy and acidic. Vascular plant species were determined, with respective life forms and canopy coverage areas. The total number of species when all four sites were added was 135, and the number of species per island varied from 2 to 32. The areas of the 214 soil islands varied from 0.015 to 91.9 m², totaling 568 m² in the four sites. Monocotyledon families were dominant, essentially Velloziaceae, as well as Orchidaceae, Bromeliaceae, Amaryllidaceae and Cyperaceae. Among the eudicotyledons, dominant families were mainly Clusiaceae, Asteraceae and Melastomataceae. The biological spectra revealed that phanerophytes and hemicryptophytes predominated among the life forms, while chamaephytes had the largest coverage area. Epilithic and desiccant chamaephytes composed the most conspicuous interspecific associations, and were probably related to early successional processes. Sites closest to one another were not the most similar in structure, indicating that other factors more relevant than distance might be involved in the abundance of species in space.