1Analytical Science and Technology, Generics, IPDO, Dr. Reddy's Laboratories, Bachupally, Hyderabad-500090, India
2Department of Chemistry, GSS, GITAM University, Visakhapatnam – India – AP – 530045
3Research Fellow in Internal Medicine Department in Mayo Clinic4500 San Pablo Road, Jacksonville, Florida, 32224
A validated reverse-phase ultra-performance liquid chromatography (UPLC) method has been developed for the precise determination of impurities in Clidinium Bromide (CDB) and Chlordiazepoxide Hydrochloride (CDH) Capsules. This study focuses on the separation of impurities, namely Benzylic acid (BZY) related to Clidinium, Chlordiazepoxide Related Compound A (CDRC-A), and Chlordiazepoxide Related Compound C (CDRC-C). The Water’s H-Class UPLC system, equipped with a PDA Detector, was employed with a 15μL loop size, operating at a detection wavelength of 215 nm in gradient mode with a flow rate of 0.3 mL/min, resulting in a total run time of 55 min. The chromatographic separation utilized a Waters Acquity UPLC BEH C18 column (150 mm × 2.1 mm i.d., 1.7 μm particle size) at a column temperature of 55°C. The method demonstrated robustness and accuracy with retention times for CDB (4.4), BZY (5.2), CDRC-A (8.5), CDH (12.1), and CDRC-C (33.8). The % Accuracy at 100% for CDB is 98.2, BZY is 0.0765, CDRC-A is 0.1350, CDH is 98.2 and CDRC-C is 101.0 respectively. LOQ values for CDB is 0.0756, BZY is 0.0765, CDRC-A is 0.1464, CDH is 0.0749 and CDRC-C is 0.1932. Linear responses were observed for all impurities, including CDB and CDH. This validated UPLC method is deemed more appropriate to regular QC analysis as well as Stability study analysis of CDB and CDH Capsules formulations.
CDB, CDH, RP-UPLC, Retention time, Impurities, Validation
