An Experimental Design Approach for Impurity Profiling of Valacyclovir-Related Products by RP-HPLC

Abstract

Impurity profiling has become an important phase of pharmaceutical research where both spectroscopic and chromatographic methods find applications. The analytical methodology needs to be very sensitive, specific, and precise which will separate and determine the impurity of interest at the 0.1% level. Current research reports a validated RP-HPLC method to detect and separate valacyclovir-related impurities (Imp-E and Imp-G) using the Box-Behnken design approach of response surface methodology. A gradient mobile phase (buffer: acetonitrile as mobile phase A and acetonitrile: methanol as mobile phase B) was used. Linearity was found in the concentration range of 50–150 μg/mL. The mean recovery of impurities was 99.9% and 103.2%, respectively. The %RSD for the peak areas of Imp-E and Imp-G were 0.9 and 0.1, respectively. No blank interferences at the retention times of the impurities suggest the specificity of the method. The LOD values were 0.0024 μg/mL for Imp-E and 0.04 μg/mL for Imp-G and the LOQ values were obtained as 0.0082 μg/mL and 0.136 μg/mL, respectively, for the impurities. The S/N ratios in both cases were within the specification limits. Proper peak shapes and satisfactory resolution with good retention times suggested the suitability of the method for impurity profiling of valacyclovir-related drug substances.

Experimental design optimization of RP-HPLC method for simultaneous estimation of metsulfuron-methyl, chlorantraniliprole and chlorimuron-ethyl residues in stems of Oryza sativa

“…The purpose of this research was to develop and validate chemometrically optimized simple, precise and reliable RP-HPLC method for simultaneous determination of three pesticide residues of metsulfuron-methyl, chlorantraniliprole and chlorimuron-ethyl in stems of Oryza sativa. In earlier studies, chemometrics for the optimization of analytical method development was successfully applied [18,19]. In the present research, the results of the chemometric tools such as response surface methodology and ANOVA were tested for optimization of each factor.…”

Method Development, Validation and Stress Studies of Valacyclovir HCl in Bulk and Pharmaceutical Dosage Form Using RP-HPLC

“…igh Performance Liquid Chromatography is one of the widely used analytical techniques used for the separation, identification and quantification of components in a mixture [1][2][3] . This technique is mostly suitable for non-volatile compounds, thermally unstable compounds and compounds having high molecular weights.…”

CHEMOMETRICS ASSISTED VALIDATED HPLC METHOD DETECTING SEASONAL VARIANCES OF SECONDARY METABOLITES OF Camellia sinensis CONSIDERING THE ABIOTIC STRESSES

“…As a measure of robustness of the method, deliberate alterations in the flow rate (0.5 mL/min and 1.5 mL/min) was made to evaluate the impact of the method. The tailing factor, %RSD of asymmetry and retention time of standard should not be more than 2% due to the intentional alterations in the flow rate (Katakam et al, 2014). Abiotic factors and secondary metabolites: TV 25 variety of tea used as the research material has been grown in the tea garden of IIT Kharagpur.…”