Otimização evalidação de métodos analíticos para a determinação simultânea de tuberculostáticos (4-FDC) por CLAE/DAD e CLUE/ DAD

Tuberculosis is a serious disease, but curable in practically 100% of new cases, since complied the principles of modern chemotherapy. Isoniazid (ISN), Rifampicin (RIF), Pyrazinamide (PYR) and Chloride Ethambutol (ETA) are considered first line drugs in the treatment of tuberculosis, by combining the highest level of efficiency with acceptable degree of toxicity. Concerning USP 33 - NF28 (2010) the chromatography analysis to 3 of 4 drugs (ISN, PYR and RIF) last in average 15 minutes and 10 minutes more to obtain the 4th drug (ETA) using a column and mobile phase mixture different, becoming its industrial application unfavorable. Thus, many studies have being carried out to minimize this problem. An alternative would use the UFLC, which is based with the same principles of HPLC, however it uses stationary phases with particles smaller than 2 μm. Therefore, this study goals to develop and validate new analytical methods to determine simultaneously the drugs by HPLC/DAD and UFLC/DAD. For this, a analytical screening was carried out, which verified that is necessary a gradient of mobile phase system A (acetate buffer:methanol 94:6 v/v) and B (acetate buffer:acetonitrile 55:45 v/v). Furthermore, to the development and optimization of the method in HPLC and UFLC, with achievement of the values of system suitability into the criteria limits required for both techniques, the validations have began. Standard solutions and tablets test solutions were prepared and injected into HPLC and UFLC, containing 0.008 mg/mL ISN, 0.043 mg/mL PYR, 0.030 mg.mL-1 ETA and 0.016 mg/mL RIF. The validation of analytical methods for HPLC and UFLC was carried out with the determination of specificity/selectivity, analytical curve, linearity, precision, limits of detection and quantification, accuracy and robustness. The methods were adequate for determination of 4 drugs separately without interfered with the others. Precise, due to the fact of the methods demonstrated since with the days variation, besides the repeatability, the values were into the level required by the regular agency. Linear (R> 0,99), once the methods were capable to demonstrate results directly proportional to the concentration of the analyte sample, within of specified range. Accurate, once the methods were capable to present values of variation coefficient and recovery percentage into the required limits (98 to 102%). The methods showed LOD and LOQ very low showing the high sensitivity of the methods for the four drugs. The robustness of the methods were evaluate, facing the temperature and flow changes, where they showed robustness just with the preview conditions established of temperature and flow, abrupt changes may influence with the results of methods

Desenvolvimento e testes de software de um receptor de GPS para uso espacial

Spacecraft move with high speeds and suffer abrupt changes in acceleration. So, an onboard GPS receiver could calculate navigation solutions if the Doppler effect is taken into consideration during the satellite signals acquisition and tracking. Thus, for the receiver subject to such dynamic cope these shifts in the frequency signal, resulting from this effect, it is imperative to adjust its acquisition bandwidth and increase its tracking loop to a higher order. This paper presents the changes in the GPS Orion s software, an open architecture receiver produced by GEC Plessey Semiconductors, nowadays Zarlink, in order to make it able to generate navigation fix for vehicle under high dynamics, especially Low Earth Orbit satellites. GPS Architect development system, sold by the same company, supported the modifications. Furthermore, it presents GPS Monitor Aerospace s characteristics, a computational tool developed for monitoring navigation fix calculated by the GPS receiver, through graphics. Although it was not possible to simulate the software modifications implemented in the receiver in high dynamics, it was observed that the receiver worked in stationary tests, verified also in the new interface. This work also presents the results of GPS Receiver for Aerospace Applications experiment, achieved with the receiver s participation in a suborbital mission, Operation Maracati 2, in December 2010, using a digital second order carrier tracking loop. Despite an incident moments before the launch have hindered the effective navigation of the receiver, it was observed that the experiment worked properly, acquiring new satellites and tracking them during the VSB-30 rocket flight.