Sorption and preconcentration of metal ions in ethanol solution with a silica gel surface chemically modified with benzimidazole

The adsorption isotherms of MCl(2) (M = Mn, Ni, Cu, Zn and Cd) and FeCl3 by silica gel chemically modified with benzimidazole molecules (= SI(CH2)(3)-NC7H5N) were studied in ethanol solution at 298 K. A column made of modified silica was used to adsorb and preconcentrate the above metal ions from ethanol solution. Elution was done with 0.1 M hydrochloric acid in an ethanol/water mixture having a mole fraction of water of 0.8. The material was applied in the preconcentration of metal ions from commercial ethanol normally used as engine fuel.

ESR STUDY OF CUCL2 ADSORBED ON A CHEMICALLY-MODIFIED SILICA-GEL SURFACE WITH BENZIMIDAZOLE MOLECULE

The ESR spectrum of CuCl2 adsorbed onto a silica gel surface chemically modified with the benzimidazole molecule showed that the surface complex has an octahedral symmetry with tetragonal distortion. The measured ESR parameters were g(parallel to) = 2.287, g(perpendicular to) = 2.062, A(parallel to) = 153 G and superhyperfine splitting A(N) = 15 G. The fit of the theoretical expressions to the experimental data was very reasonable. The effective spin orbit coupling constant for Cu2+ was reduced from its normal free ion value of lambda = -828 cm(-1) by as much as 30%. This reduction of lambda is normal in the solid state and in frozen solution complexes.

Structure of cobalt (II) perchlorate adsorbed on silica gel surface chemically modified with benzimidazole molecule

Covalently attached benzimidazole molecules on silica gel surface, ≡SiL (where L = N-propyl-benzimidazole), adsorbs Co(ClO4)2 from non-aqueous solvent by forming a surface complex according to the reaction: m ≡SiL + Co(ClO4)2 → (≡SiL)mCo(ClO4)2. The equilibrium constant and the adsorption capacity, determined by applying the Langmuir equation were b = 3.0 × 103 L mol-1 and Ns= 0.098 × 10-3 mol g-1, respectively. The metal is bonded through the nitrogen atom and the perchlorate ion is not coordinated. The ESR study indicated that the complex has essentially an octahedral geometry with tetragonal distortion, with the electrons of the four nitrogen atoms interacting with the cobalt central metal ion in the equatorial plane. Only one complex species was detected on the surface.

Structure of copper complexes adsorbed on a silica gel surface chemically modified with benzimidazole

Silica gel having a particle size between 0.2 and 0.05 mm and a specific surface area, S BET = 473 m 2 g -1, was chemically modified with benzimidazole. Adsorption isotherms of CuX 2 (X = Cl, Br or ClO 4) from ethanol and acetone solutions were studied at 298 K. The metal is bonded to the surface through the free nitrogen atom of the attached benzimidazole. The average number of ligands co-ordinated to the central metal ion was shown to depend on the solid surface loading by the solute. At low loading the electronic and ESR spectral parameters indicated that the copper ion is in a distorted-tetragonal symmetry field.

Electrochemical Redox Behavior of Omeprazole Using a Glassy Carbon Electrode

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Theoretical study of omeprazole behavior: Racemization barrier and decomposition reaction

omeprazole is a substituted benzimidazole which suppresses gastric-acid secretion by means of H+, K+-ATPase inhibition. It is an optically active drug with the sulfur of the sulfoxide being the chiral center. This pro-drug can be easily converted into its respective sulfenamide at low pH. In this work, omeprazole has been studied in relation to racemization barrier and decomposition reaction. Quantum chemistry coupled to PCA chemometric method were used to find all minimum energy structures. Conformational analysis and calculation of racemization barriers were carried out by PM3 semiempirical method (Gaussian 98). The average racemization energy barrier for all minimum energy structures (43.56 kcal mol(-1)) can be related to the velocity constant in Eyring's equation. The enormous half-life time at 100 degrees C (9.04 x 10(4) years) indicates that the process cannot be observed in human time scale. on the other hand, the difference of free energy change (Delta(Delta G) = -266.78 kcal mol(-1)) for the decomposition reaction shows that the process is favorable to the sulfenamide formation. The highly negative Delta(Delta G) obtained for the decomposition reaction shows that this process is extremely exothermic. This result explains why omeprazole decomposes and does not racemize. (C) 2008 Wiley Periodicals, Inc.

Determination of pesticide residues in coconut water by liquid-liquid extraction and gas chromatography with electron-capture plus thermionic specific detection and solid-phase extraction and high-performance liquid chromatography with ultraviolet detection

Two simple methods were developed to determine, 11 pesticides in coconut water, a natural isotonic drink rich in salts, sugars and vitamins consumed by the people and athletes. The first procedure involves solid-phase extraction using Sep-Pak Vac C-18 disposable cartridges with methanol for elution. Isocratic analysis was carried out by means of high-performance liquid chromatography with ultraviolet detection at 254 nm to analyse captan, chlorothalonil, carbendazim, lufenuron and diafenthiuron. The other procedure is based on liquid-liquid extraction with hexane-dichloromethane (1:1, v/v), followed by gas chromatographic analysis with effluent splitting to electron-capture detection for determination of endosulfan, captan, tetradifon and trichlorfon and thermionic specific detection for determination of malathion, parathion-methyl and monocrotophos. The methods were validated with fortified samples at different concentration levels (0.01-12.0 mg/kg). Average recoveries ranged from 75 to 104% with relative standard deviations between 1.4 and 11.5%. Each recovery analysis was repeated at least five times. Limits of detection ranged from 0.002 to 2.0 mg/kg. The analytical procedures were applied to 15 samples and no detectable amounts of the pesticides were found in any samples under the conditions described. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Evaluation of a larval development assay for the detection of anthelmintic resistance in Ostertagia circumcincta

Two experiments were carried out to evaluate a larval development assay for the detection of anthelmintic resistance in O. circumcincta. In Experiment I, the dose responses to levamisole (LEV), thiabendazole (TBZ) and ivermectin (IVM) of 8 isolates of O. circumcincta were measured 34 days after infection (DAI). Four of these isolates were shown to be resistant to 1 or more anthelmintics. With 2 exceptions, all isolates considered to be resistant had higher LD50 values than the susceptible isolates for that anthelmintic. One exception was isolate RM8, which was considered to be resistant to all 3 anthelmintics based on faecal egg count reduction tests in goats, but the LD50 value for LEV did not differ from that for the susceptible isolates. The other exception was an isolate considered to be susceptible to TBZ which had a relatively high LD50 value. In an unrelated trial that was prompted by this finding, this isolate was confirmed to be benzimidazole-resistant. Isolate RM8 and an isolate susceptible to all 3 anthelmintics (SK2) were used in the second experiment, which was conducted to monitor changes in the LD50 values of LEV, TBZ and IVM over time following a single infection of 35 000 infective larvae in young sheep. Faecal samples were collected weekly from 24 to 115 DAI. With all 3 anthelmintics, the LD50 values increased with time to a peak around 50-60 DAI, and then declined to levels similar to those observed soon after patency. This trend was consistent for both isolates. The highest mean LD50 values for isolates SK2 for IVM and TBZ and RM8 for IVM and RM8, respectively, were 1.7 and 1.8 times, and 2.2 and 2.9 times higher than the initial mean LD50 values. There was a clear distinction in LD50 values between isolates at each sampling day for both IVM and TBZ. However, as a consequence of the changes in LD50 values with time, the peak LD50 values of IVM for isolate SK2 were higher than the minimum LD50 values of isolate RM8. As there was no apparent difference in LEV efficacy between these 2 isolates, the data were pooled. The highest mean LD50 value was 2.3 times higher than the initial LD50 value. (C) 1997 Australian Society for Parasitology.

Haemonchus contortus: A multiple-resistant Brazilian isolate and the costs for its characterization and maintenance for research use

The aim of this work was to determine the resistance level of Haemonchus contortus isolated from the Santa Inês flock of the Embrapa (Brazilian government's Agricultural Research Company), Southeast Livestock Unit (CPPSE), as well as to determine costs of characterizing and maintaining this isolate in host donors. Forty-two male Santa Inês lambs were experimentally infected with 4000 H. contortus infective larvae of the field isolate of CPPSE, called Embrapa2010, and divided into six treatment groups, which received triclorfon, albendazol plus cobalt sulfate, ivermectin, moxidectin, closantel and levamisole phosphate, as well as a negative control group (water). Egg per gram (EPG) counts were performed at 0, 3, 7, 10 and 14. days post treatment when the animals were slaughtered for parasite count. The data were analyzed using the RESO statistical program, considering anthelmintic resistance under 95% of efficacy. EPG and worm count presented a linear and significant relation with 94% determination coefficient. The susceptibility results obtained by RESO through both criteria (EPG and worm count) were equal, except for closantel, showing that the isolate Embrapa2010 is resistant to benzimidazoles, macrocyclic lactones and imidazothiazoles. The need of a control group did not appear to be essential since the result for susceptibility in the analyses with or without this group was the same. Suppression in egg production after treatment did not occur in the ivermectin and moxidectin groups. In the control group, the establishment percentage was just 12.5 because of the low number of third-stage larvae, resistance (innate and infection immunity) of the animals studied plus good nutrition. Drug classes presented similar efficacy between adults and immature stages. The costs for isolate characterization were calculated for 42 animals during 60. days. The total cost based on local market rates was approximately US$ 8000. The precise identification of Brazilian isolates and their establishment in host donors would be useful for laboratorial anthelmintic resistance diagnoses through in vitro tests, which has an annual cost of approximately US$ 2500 for maintenance in host donors. © 2012 Elsevier B.V.

Estudo dos compostos voláteis da decomposição térmica dos anti-helmínticos Albendazol e Mebendazol

The albendazole and mebendazole drugs are benzimidazole derivatives and belong to the anthelmintic class. These drugs are particularly recommended for the treatment against worms present in the gastrointestinal tract of animals and humans, by acting directly on the worm metabolism. The need for thermally study drugs is related to all the parameters that these analyzes include: presence or absence of polymorphs, possible changes in the crystallinity of the drugs, as well as the quality control during the manufacturing process thereof. In this study the thermal behavior of anthelmintic albendazole and commercial mebendazole and its recrystallisation in organic solvents, such as acetic acid and formic acid in dimethylformamide to mebendazole, and albendazole were studied using TG-DSC techniques, TG-FTIR, FTIR and XRD. TG-DSC techniques were used so it could collect information about the thermal stability of the compounds steps for thermal decomposition process and also prove its melting temperature. For recrystallization of drugs in organic solvents, the TG-DSC curves were analyzed to compare and determine that the occurrence of polymorphs. The coupled TG-FTIR technique allowed the analysis of volatile products which were released during the thermal decomposition of the commercial mebendazole. The absorption spectroscopy in the infrared region was performed to mebendazole, and albendazole in order to show the difference in functional groups of both, comparing the spectra with commercial drugs and see if there was recrystallized changes in the absorption band where the drug was recrystallized or when heated. The diffraction technique by powder X-ray method was used for comparison of the crystal structures of commercial drugs and recrystallization in organic solvents to identify changes in crystallinity both, which might suggest the formation of polymorphs

Polymeric and solid lipid nanoparticles for sustained release of carbendazim and tebuconazole in agricultural applications

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