A stability-indicating liquid chromatographic (LC) method was studied for the determination of paliperidone in osmoticcontrolled release oral delivery system (OROS) tablets. A tablet extraction procedure was developed by testing the efficiency of solvents (water, HCl, NaOH, acetonitrile, methanol) and techniques (ultrasonic bath, magnetic stirrer), and evaluating the release of the drug with respect to time. A forced degradation study was conducted to demonstrate the stability-indicating power of the method. Chromatographic separation was achieved using an isocratic elution in a reversed-phase system with a mobile phase prepared from a mixture of phosphate buffer and acetonitrile. The use of an ultrasonic bath demonstrated paliperidone release from OROS tablets in a total time of 60 min. Verifying the efficiency of the chromatographic procedure, the theoretical plates (N = 12634.21) and tailing factor (tf = 1.31) were constant during repeated injections. The retention time of paliperidone was 4.8 min, and the method was validated within the concentration range of 10-50 µg mL −1 (r = 0.9999). Adequate reproducibility (RSD% = 0.30-0.59), interday precision (RSD% = 1.81), and accuracy were obtained. The proposed method was successfully applied to paliperidone determination in the presence of degradation products, and an efficient extraction procedure from the OROS tablets was developed.
Recebido em 1/11/10; aceito em 14/5/11; publicado na web em 22/7/11 Doripenem was characterized through physicochemical and spectroscopic techniques, as well as thermal analysis. TLC (Rf = 0.62) and HPLC (rt = 7.4 min) were found to be adequate to identify the drug. UV and infrared spectra showed similar profile between doripenem bulk and standard. The 1 H and 13 C NMR analysis revealed chemical shifts that allowed identifying the drug. Thermal analysis demonstrated three steps with mass loss, at 128, 178 and 276 o C. The work was successfully applied to qualitative analysis of doripenem, showing the reported methods can be used for physicochemical characterization of doripenem.
Summary.A stability-indicating liquid chromatographic (LC) method with UV detection was developed for the determination of doripenem in the marketed formulation (Doribax ® 500 mg, powder for injection). A forced degradation study was conducted according to available guidelines and main references. Thermal, oxidizing, acidic and basic stress conditions were assayed to show the stability-indicating power of the method. Chromatographic separation was achieved using an isocratic elution method in a reversed-phase system using a mobile phase prepared from phosphate buffer and acetonitrile. Extensive degradation was observed under thermal, oxidative and basic treatment, and the products formed were detected without interference in the analysis of doripenem. To verify the efficiency of chromatographic run, the system suitability was studied. The theoretical plates (N = 5498.3) and tailing factor (tf = 0.951) were constant during repeated injections. The retention time of doripenem was 7.35 min and the method was validated within the concentration range 5-50 μg mL −1 (r = 0.999). Adequate results were obtained that indicate repeatability (RSD % = 1.03-1.37), inter-day precision (RSD % = 0.51) and accuracy. In comparison to spectrophotometric and microbiological methods, statistical analysis showed no significant difference between the obtained results. The proposed method was successfully applied to doripenem quantification, showing it is applicable to determine the antibiotic in the presence of degradation products and also that is a reliable method for routine analysis.
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