Lígia Maria Moreira de Campos

Bioleaching of zinc and nickel from silicates using Aspergillus niger cultures

In this work, we investigated the role of bacteria from the genera Bacillus and Pseudomonas and fungi from the genera Aspergillus and Penicillium in the leaching process of two different silicates (calamine and garnierite). Since the results obtained with A. niger were better than those with different bacteria, a more detailed investigation of the leaching process with this microorganism was conducted. Moreover, although it is clear that the citric acid generated by fungi could be an important leaching agent acting in the solubilization of the used silicates, other products of metabolism could be involved. Related to this, the results obtained with chemical leaching using low concentrations of citric acid (lower than 10 mM) showed, for both calamine and garnierite, that the respective dissolution of zinc and nickel was much lower when compared to those processes in which cultures or supernatant liquor of A. niger cultures were used and in which the maximum concentration of citric acid was 8 mM. The results obtained also suggest that the type of mineral (and/or the metal present in it) presents a different susceptibility to the bioleaching process and also demonstrate that depending of the situation, the presence of the fungi cells seem to improve the leaching process. From a practical point of view, the high yield rate of extracting metals from silicates obtained by using for example, supernatant liquors of A. niger cultures, is noteworthy. This bioleaching process present two advantages as compared to conventional chemical leaching processes: (a) the very low concentrations of organic compounds present in such a situation represent a lower ecological risk; and (b) even with a lower final yield, the economical cost of a such process. Both characteristics could facilitate its industrial application.

Carbohydrate carbamate coated onto microporous silica: Application to chiral analysis of commercial pharmaceutical drugs

The enantioselectivity of a series of chiral analytes was examined on tris-(3,5-dimethylphenyl carbamate) coated onto microporous APS-silica. The effects of the nature of the carbohydrate, the weight ratio of carbamate/support and the type of alcohol present in the mobile phase were investigated. Among the chiral analytes examined, propanolol showed an extremely good resolution. The resolution of tetramisole was optimized and the method developed was shown to be suitable for analysis of the drug in commercial tablets and in a suspension.

Validation and statistical analysis of two high performance liquid chromatography methods for the determination of indinavir sulfate raw material and capsules

Two high performance liquid chromatography (HPLC) methods for the quantitative determination of indinavir sulfate were tested, validated and statistically compared. Assays were carried out using as mobile phases mixtures of dibutylammonium phosphate buffer pH 6.5 and acetonitrile (55:45) at 1 mL/min or citrate buffer pH 5 and acetonitrile (60:40) at 1 mL/min, an octylsilane column (RP-8) and a UV spectrophotometric detector at 260 nm. Both methods showed good sensitivity, linearity, precision and accuracy. The statistical analysis using the t-student test for the determination of indinavir sulfate raw material and capsules indicated no statistically significant difference between the two methods.

Development and validation of an alternative titration method for the determination of sulfate ion in indinavir sulfate

A simple and rapid precipitation titration method was developed and validated to determine sulfate ion content in indinavir sulfate raw material. 0.1 mol L-1 lead nitrate volumetric solution was used as titrant employing potentiometric endpoint determination using a lead-specific electrode. The United States Pharmacopoeia Forum indicates a potentiometric method for sulfate ion quantitation using 0.1 mol L-1 lead perchlorate as titrant. Both methods were validated concerning linearity, precision and accuracy, yielding good results. The sulfate ion content found by the two validated methods was compared by the statistical t-student test, indicating that there was no statistically significant difference between the methods.

Desenvolvimento e validação de método por cromatografia líquida de alta eficiência para determinação simultânea das impurezas timina e timidina na matéria-prima estavudina

A HPLC method was developed to quantify thymine and thymidine impurities in stavudine bulk drug. The separation was carried out in isocratic mode using methanol/water (20:80) as mobile phase, a C18 column and UV detection at 266 nm. The method provided selectivity based on peak purities and resolution among peaks. It was linear over the range of 0.5-5.0 µg/mL. The quantitation limits were 0.021 µg/mL for thymine and 0.134 µg/mL for thymidine. The average accuracies of three concentrations ranged from 97.06 to 102.61% and precision was close to 1%. The method showed robustness, remaining unaffected by deliberate variations in relevant parameters.

Validação de metodologia para doseamento e estudo de equivalência farmacêutica de comprimidos de lamivudina 150 mg

Lamivudine is a drug used in the treatment of types 1 and 2 HIV infections. It has been widely used in Brazil, in public programs of the Health Ministry. This work reports lamivudine assay methodologies, which have been developed and validated. Pharmaceutical equivalency studies were also performed for lamivudine tablets. Physical and physicochemical parameters of immediate release reference and test tablets of four different laboratories (G, A, B and C) were evaluated. The proposed analytical method, high performance liquid chromatography, presented satisfactory precision, accuracy, linearity and specificity. Batches from laboratories G, A and B showed appropriate results in all tests to which they were submitted. Tablet batches from laboratory G (reference) showed similar dissolution profile and fast dissolution rate. The products A and B showed differences between their batches, in regards to the dissolution rates at the initial profile. However at the end of the profile they reached similar release to the reference, product G. Therefore they can be considered pharmaceutical equivalents to the reference product. Batches of product from laboratory C showed much more differences with reduced dissolution presenting no appropriate quality for human consumption.

Determinação de lamivudina, estavudina e nevirapina, em comprimidos, por cromatografia líquida de alta eficiência

A high performance liquid chromatography method was developed to quantify lamivudine, stavudine and nevirapine combined in tablets. The separation was carried out in less than 10 min using a phosphate buffer of pH 3.0 and acetonitrile (75:25, v/v) as mobile phase, a LiChrospher ODS column and UV detection at 266 nm. The method was linear over the range of 15-135 µg/mL (lamivudine), 4-36 µg/mL (stavudine) and 20-180 µg/mL (nevirapine). The accuracy ranged from 98.56 to 102.04% and intra-day and inter-day precision was less than 1% for the three drugs. The method showed robustness, remaining unaffected by deliberate variations in relevant parameters.