3. RESULTS AND DISCUSSION
3.1. Method development and optimization
The main criterion is to develop successful HPLC method for the determination of FVS and its degradation product. The developed method should be able to determine FVS and its degradation product in a single run. This method should be accurate, reproducible, robust, stability indicating, free of interference from degradation products and straight forward enough for routine use in quality control laboratory.
Regulatory agencies recommend the use of stability-indicating methods for the analysis of stability of samples. Thus, stress studies are required in order to generate the stressed samples, method development, and method validation [29-33]. In order to separate FVS and degradation …show more content…
The retention time of FVS was 4.50 ± 0.05 min (Fig. 1). This mobile phase gave good resolution for the separation of FVS and its degradation products and was selected for the proposed stability-indicating method. The optimized conditions of the HPLC method were validated for the analysis of FVS in capsule formulations and application for QC. Fig. 1 shows a typical chromatogram obtained by the proposed RP-HPLC method, demonstrating the resolution of the symmetrical peak corresponding to FVS. The retention time observed (4.5 min) allows a fast determination of the drug, which is suitable for QC …show more content…
The increased concentration of acid increased the formation of the main degradation product, and the area of the FVS peak decreased drastically (Fig. 2(a), (b), (c), 2-(a)). A regular decrease in the concentration of intact FVS with increasing time intervals was observed. During the acidic degradation major degradation product was observed at 6.54mins without interfering the elution of drug peak (FVS=4.5mins) (Fig. 3(a), (b), (c), 2-(a)). At the selected temperature (50, 60, 70 80°C) the acid degradation of FVS processes first-order kinetics (Fig. 5(a)). The apparent first order degradation rate constant and the half life at each temperature are shown in Table 5. The influence of temperature on the reaction rate constant (kobs) in 0.1MHCl was given by the Arrhenius
3.1. Method development and optimization
The main criterion is to develop successful HPLC method for the determination of FVS and its degradation product. The developed method should be able to determine FVS and its degradation product in a single run. This method should be accurate, reproducible, robust, stability indicating, free of interference from degradation products and straight forward enough for routine use in quality control laboratory.
Regulatory agencies recommend the use of stability-indicating methods for the analysis of stability of samples. Thus, stress studies are required in order to generate the stressed samples, method development, and method validation [29-33]. In order to separate FVS and degradation …show more content…
The retention time of FVS was 4.50 ± 0.05 min (Fig. 1). This mobile phase gave good resolution for the separation of FVS and its degradation products and was selected for the proposed stability-indicating method. The optimized conditions of the HPLC method were validated for the analysis of FVS in capsule formulations and application for QC. Fig. 1 shows a typical chromatogram obtained by the proposed RP-HPLC method, demonstrating the resolution of the symmetrical peak corresponding to FVS. The retention time observed (4.5 min) allows a fast determination of the drug, which is suitable for QC …show more content…
The increased concentration of acid increased the formation of the main degradation product, and the area of the FVS peak decreased drastically (Fig. 2(a), (b), (c), 2-(a)). A regular decrease in the concentration of intact FVS with increasing time intervals was observed. During the acidic degradation major degradation product was observed at 6.54mins without interfering the elution of drug peak (FVS=4.5mins) (Fig. 3(a), (b), (c), 2-(a)). At the selected temperature (50, 60, 70 80°C) the acid degradation of FVS processes first-order kinetics (Fig. 5(a)). The apparent first order degradation rate constant and the half life at each temperature are shown in Table 5. The influence of temperature on the reaction rate constant (kobs) in 0.1MHCl was given by the Arrhenius