Reversed-Phase UHPLC Enantiomeric Separation of Rasagiline Salts Using a Chiralpak^® AGP Column

Area of Science:

• Analytical Chemistry
• Pharmaceutical Analysis

Background:

• Rasagiline is a crucial pharmaceutical agent requiring enantiomeric purity.
• Existing methods for rasagiline enantiomer separation often utilize normal-phase chiral columns, which can be less efficient.
• Development of rapid and robust analytical methods is essential for pharmaceutical quality control.

Purpose of the Study:

• To develop and validate a rapid ultra-high performance liquid chromatographic (UHPLC) enantiomeric reversed-phase separation method for rasagiline.
• To provide an alternative to normal-phase chiral chromatography for rasagiline isomer analysis.
• To establish a method suitable for quality control during pharmaceutical manufacturing.

Main Methods:

• Utilized a Chiralpak® AGP column (50 mm × 2.1 mm, 5 μm) as the stationary phase.
• Employed an isocratic mobile phase consisting of ammonium acetate and isopropyl alcohol (90:10, v/v) at a flow rate of 0.6 mL/min.
• Validated the method according to International Council on Harmonization (ICH) guidelines, including precision, linearity, accuracy, and robustness.

Main Results:

• Achieved rapid enantiomeric separation of rasagiline mesylate and its tartrate salts.
• Established a detection limit of 0.06 μg/mL and a quantification limit of 0.2 μg/mL for rasagiline enantiomers.
• Demonstrated compatibility with UHPLC-MS and confirmed separation via specific optical rotation measurements.

Conclusions:

• The developed UHPLC method offers a fast and efficient alternative for rasagiline enantiomer separation.
• This validated method is suitable for in-process control and quality assurance in the pharmaceutical industry.
• The method facilitates the production of optically pure rasagiline, ensuring drug efficacy and safety.