Simple and Reliable Gas Chromatography Method for the Determination of 3-Quinuclidinol Content in Solifenacin Succinate Drug Substance

Abstract

A simple and reliable gas chromatography method has been developed and validated for the determination of 3-quinuclidinol content in solifenacin succinate drug substance, using dimethyl- sulfoxide (DMSO) as internal standard (IS). Efficient chromatographic separation was achieved on DB-Wax, 15 m long with 0.53 mm i.d., 1.0 µm particle diameter column consists with 100% polyethylene glycol as stationary phase including carrier gas as Helium. The analyte and internal standard were extracted in chloroform and monitored by flame ionization detector. The performance of the method was assessed by evaluating specificity, precision (repeatability, reproducibility), linearity, robustness and accuracy. No interference of organic solvents used in the synthesis was observed. The proposed method has a potential application to drug substances which may contains 3-quinuclidinol. The limits of detection (LOD) and limits of quantification (LOQ) established for 3-quinuclidinol, 40 µg g -1 and 120 µg g -1 respectively. The correlation coefficient value of linearity experiment is 0.9997. The average recovery for 3-quinuclidinol is 100.8%. The results proves that the validated method was suitable for determining 3-quinuclidinol content and method can be successfully applied for the routine analysis of solifenacin succinate drug substance.