Rasagiline hemitartrate: Synthesis, characterization and RP-HPLC validation for its estimation in bulk form

Objectives

To develop a reverse phase high performance liquid chromatographic method for validation and quantitative estimation of the synthesized drug rasagiline hemitartrate in bulk form.

Methods

Rasagiline hemitartrate was synthesized and characterized by spectral (Infrared, Proton Nuclear Magnetic Resonance and Mass) as well as elemental analysis. Chromatographic separation was conducted on Agilent TC-C18 (250 × 4.6 mm, 5 μm) column at ambient temperature using mixture of 20 mM potassium dihydrogen orthophosphate buffer (pH 7.0): methanol and acetonitrile in the ratio (30:30:40 v/v) as a mobile phase and at a flow rate of 1.0 mL/min, while UV detection was performed at 285 nm. In addition to LOD and LOQ, other analytical parameters viz., linearity, precision, accuracy, ruggedness and robustness were detected by following the ICH (International Conference on Harmonization) guidelines.

Results

The retention time for rasagiline hemitartrate was found to be 4.30 ± 0.05 min. The method was found to be linear in the range of 10–50 μg/mL. The limit of detection and quantization for rasagiline hemitartrate are found to be 0.651 and 1.972 μg/mL respectively. Analytical recovery was 100.47%. The percentage RSD for precision and accuracy of the method was found to be less than 2%. Correlation coefficient was found to be 0.9952.

Conclusion

In this study, simple, sensitive, accurate and reliable RP-HPLC method was developed and validated as per the ICH guidelines for the determination of the synthesized drug rasagiline hemitartrate in bulk form.