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

Katakam P, Dey B, Hwisa NT, Assaleh FH, Chandu BR, Singla RK, Mitra A - Sci Pharm (2014)

Bottom Line: Linearity was found in the concentration range of 50-150 μg/mL.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.

View Article: PubMed Central - PubMed

Affiliation: Faculty of Pharmacy, University of Zawia, Az Zawiyah, Libya.

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.

No MeSH data available.


Related in: MedlinePlus

Chromatogram for the optimized method
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Figure 3: Chromatogram for the optimized method

Mentions: A validated RP–HPLC method was developed to detect and separate valacyclovir and related impurities (E and G) using the Box-Behnken design approach. The design matrix of the Box-Behnken model of the RSM and experimental runs for the optimization of chromatographic conditions are provided in Table 1. The contour plots of the percent peak area and retention time vs. flow rate, column temperature, acetonitrile (ACN), and buffer in the mobile phase are provided in Figure 2. The details of the linearity data of impurities E and G are provided in Table 3. A representative chromatogram of the optimized method is provided in Figure 3. Results of the method validation showed that the mean recovery (%) of impurity E at the specification level (50, 100, and 150 μg) was 99.9% and the mean recovery of impurity G was 103.2%. For determining the precision of the method, the values of the RSD for the areas of impurities E and G were found to be 0.9% and 0.1%, respectively.


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

Katakam P, Dey B, Hwisa NT, Assaleh FH, Chandu BR, Singla RK, Mitra A - Sci Pharm (2014)

Chromatogram for the optimized method
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4318202&req=5

Figure 3: Chromatogram for the optimized method
Mentions: A validated RP–HPLC method was developed to detect and separate valacyclovir and related impurities (E and G) using the Box-Behnken design approach. The design matrix of the Box-Behnken model of the RSM and experimental runs for the optimization of chromatographic conditions are provided in Table 1. The contour plots of the percent peak area and retention time vs. flow rate, column temperature, acetonitrile (ACN), and buffer in the mobile phase are provided in Figure 2. The details of the linearity data of impurities E and G are provided in Table 3. A representative chromatogram of the optimized method is provided in Figure 3. Results of the method validation showed that the mean recovery (%) of impurity E at the specification level (50, 100, and 150 μg) was 99.9% and the mean recovery of impurity G was 103.2%. For determining the precision of the method, the values of the RSD for the areas of impurities E and G were found to be 0.9% and 0.1%, respectively.

Bottom Line: Linearity was found in the concentration range of 50-150 μg/mL.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.

View Article: PubMed Central - PubMed

Affiliation: Faculty of Pharmacy, University of Zawia, Az Zawiyah, Libya.

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.

No MeSH data available.


Related in: MedlinePlus