Validation of analytical methodology for quantification of cefazolin sodium by liquid chromatography

A reversed-phase high performance liquid chromatography method was validated for the determination of cefazolin sodium in lyophilized powder for solution for injection to be applied for quality control in pharmaceutical industry. The liquid chromatography method was conducted on a Zorbax Eclipse Plus C18 column (250 x 4.6 mm, 5 μm), maintained at room temperature. The mobile phase consisted of purified water: acetonitrile (60: 40 v/v), adjusted to pH 8 with triethylamine. The flow rate was of 0.5 mL min-1 and effluents were monitored at 270 nm. The retention time for cefazolin sodium was 3.6 min. The method proved to be linear (r2 =0.9999) over the concentration range of 30-80 µg mL-1. The selectivity of the method was proven through degradation studies. The method demonstrated satisfactory results for precision, accuracy, limits of detection and quantitation. The robustness of this method was evaluated using the Plackett–Burman fractional factorial experimental design with a matrix of 15 experiments and the statistical treatment proposed by Youden and Steiner. Finally, the proposed method could be also an advantageous option for the analysis of cefazolin sodium, contributing to improve the quality control and to assure the therapeutic efficacy

Validation of a stability indicating capillary electrophoresis method for the determination of darunavir in tablets and comparison with the of infrared absorption spectroscopic method

Darunavir (DRV) is a protease inhibitor used in the treatment of HIV infection, which constitutes a keystone in the therapy of patients infected with this virus. There is no monograph described in official compendia. The literature provides few methods of analysis for the determination of DRV in pharmaceuticals which include TLC, IR, UPLC, HPLC, HPLC-MS, HPLC-MS/MS, but there are no reports of the use of capillary electrophoresis (CE) for the determination of this drug. Thus, this research proposed the development and validation of a CE method for the determination of DRV in tablets. The method was completely validated according to the International Conference on Harmonization guidelines, showing linearity, selectivity, precision, accuracy and robustness. The migration was achieved in less than 1 minute using fused-silica uncoated capillary with an id of 50 μm and total length of 21 cm and voltage of +20 kV. The sample injection was performed in the hydrodynamic mode. The method was linear over the concentration range of 50-200 μg mL-1 with correlation coefficient 0.9998 and limits of detection and quantification of 7.29 and 22.09 μg mL-1, respectively. The drug was subjected to acid, base, oxidation and photolysis degradation. Degradation products were found interfering with the assay of DRV, therefore the method can be regarded as stability indicating. The validated method is useful and appropriate for the routine quality control of DRV in tablets.

Development and validation of infrared spectroscopy method for the determination of darunavir in tabets

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Particularities in the technique of calvaria graft

Calvaria grafts provide good bone quantity for the reconstruction of the atrophic maxilla, and have lower morbidity and resorption rates when compared to iliac crest. The aim of this paper is to present the technique for obtaining a graft of the skull. Initially, the depth of the osteotomy is determined by a manually conducted bur, which establishes the limits of the structures of the skull (outer table, diploe and inner table), making the removal of bone blocks easier and safer. Thus, osteotomies of the blocks are made with greater security, avoiding the complications inherent to surgical technique. The case that will be presented it is from a male patient of 65 years who refused to submit to the iliac crest graft, opting for the calvaria, despite being bald, that is a contraindication for this treatment modality. A delicate suture associated with placement of titanium mesh to maintain the conformation of the patient's skull in the region of the bone defect, created after removal of the graft, provided a good cosmetic result at the donor site. The use of titanium mesh for re-anatomization of bone defects created in the grafts is well indicated for bald patients.

Land use and thermal comfort in the county of Ourinhos, SP

This study aims to analyze the thermal comfort in urban areas for different land uses. The ENVImet microclimatic model has been used for urban boundary layer simulation, providing the following thermal comfort indexes: PMV (Predicted Mean Vote) and PPD (Predicted Percentage of Dissatisfaction). The chosen area covers the central area in the city of Ourinhos, located in southeastern Brazilian city, with subtropical climate. Four simulations were accomplished: an area with real buildings and vegetation on site, a “grassy” area where buildings have been replaced by grass in the central area, another grassy area, known as “grass/tree”, with additional trees in, and a final area called “Park” also grassy, where trees were added all over the area. The structures which showed thermal comfort within the ISO 7730 standards were the grassy area with no trees at 9 a.m., and a paved area, as well as the park area at 3 p.m. Other situations have presented values of PMV and PPD off the limits required by the rules; they were very close to those values. The only point that presented a far cry from the comfort required was the spot in the asphalt at 9 a.m. The other situations showed PMV and PPD values not far from the limits of comfort. Only the point on the asphalt showed values far from the limit of comfort at 9 a.m.