A Rapid Novel HPLC Method for Estimation of Eight Related Compounds in Azilsartan Kamedoxomil and Identification of Degradation Compounds by Using LC-MS.
A novel, rapid, specific and stability-indicating reverse-phase high-performance liquid chromatography method was developed for the quantitative determination of related compounds, obtained from two different synthetic routes and degradation products of Azilsartan kamedoxomil (AZL). The method was developed by using a YMC-Pack pro C18 (150 × 4.6 mm, 3 µm) column with a mobile phase containing a gradient mobile phase combination. The eluted compounds were measured at wavelength 220 nm. The developed method run time was 25 min, within which AZL and its eight impurities were well separated with minimum 3.0 resolution. The drug substance was subjected to stress conditions of hydrolysis (acid, base and water), oxidation, photolysis, sunlight, 75% relative humidity and thermal degradation as per International Conference on Harmonization (ICH) prescribed stress conditions to ascertain the stability-indicating power of the method. Significant degradation was observed during acid, base, peroxide, water hydrolysis and 75% relative humidity studies. The mass balance of AZL was close to 100% in all the stress condition. The developed method was validated as per the ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness.
Department of Chemistry, Sri Krishnadevaraya University, Anantapur, AP 515 003, India MSN Laboratories Pvt Ltd, R&D Center, Analytical Research and Development, Pashamylaram, Patancheru, Medak, Telangana 502 307, India jupallisreenivas@gmail.com srinivas.j@msnlabs.com.
J
J
Sreenivasulu
Department of Chemistry, Sri Krishnadevaraya University, Anantapur, AP 515 003, India.
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Venkata Ramana
MSN Laboratories Pvt Ltd, R&D Center, Analytical Research and Development, Pashamylaram, Patancheru, Medak, Telangana 502 307, India.
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Sampath Kumar Reddy
MSN Laboratories Pvt Ltd, R&D Center, Analytical Research and Development, Pashamylaram, Patancheru, Medak, Telangana 502 307, India.
Ch V S
ChV
Nagaraju
MSN Laboratories Pvt Ltd, R&D Center, Analytical Research and Development, Pashamylaram, Patancheru, Medak, Telangana 502 307, India.
S
S
Thirumalai Rajan
MSN Laboratories Pvt Ltd, R&D Center, Analytical Research and Development, Pashamylaram, Patancheru, Medak, Telangana 502 307, India.
S
S
Eswaraiah
D001562:Benzimidazoles / Q000032:analysis* / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004340:Drug Contamination; D057230:Limit of Detection; D016014:Linear Models; D010069:Oxadiazoles / Q000032:analysis* / Q000737:chemistry*; D015203:Reproducibility of Results
D001562:Benzimidazoles; D010069:Oxadiazoles; C521273:azilsartan