A Validated Chiral HPLC Method for the Determination of Enantiomeric Purity of R-β-amino-β-(4-methoxyphenyl) Propionic Acid |
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Authors: | P Madhavan B M Rao Pravin Abhishek P R Kumar M Sreenivasulu K B Chandrasekhar |
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Institution: | (1) Analytical Research, Custom Pharmaceutical Services, Dr. Reddy’s Laboratories, Hyderabad, 500049, India;(2) Process Research, Custom Pharmaceutical Services, Dr. Reddy’s Laboratories, Hyderabad, 500049, India;(3) Department of Chemistry, J.N.T.U. College of Engineering, Anantapur, 515002, India |
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Abstract: | A normal phase chiral LC method for chiral purity evaluation of β-amino-β-(4-methoxyphenyl) propionic acid was developed on
donor–acceptor (pirkle) column. The chiral stationary phase used was a 250 × 4.6 mm (R, R) Whelk-01 with 5 μm particle size,
which was accompanied with a 1 cm long guard column. The “hybrid” pi-electron donor–acceptor based stationary phase (R, R)
Whelk-01 was found to be enantiomeric selective for (R) and (S) enantiomers of β-amino-β-(4-methoxyphenyl) propionic acid
with a resolution >2.5. The concentration of 2-propanol and TFA in the mobile phase plays an important role on the chrmatographic
efficiency and resolution between the enantiomers. The limit of detection and limit of quantification of (S) enantiomer was
0.3 and 1.0 μg mL-1 for 20 μL injection volume. The percentage RSD of the peak area of six replicate injections of (S) enantiomer at LOQ concentration
was 4.5. The percentage recovery of (S) enantiomer from (R) enantiomer samples ranged from 92 to 100. The test solution was
observed to be stable up to 24 h after the preparation. The developed method was also checked by different analysts and on
different lots of columns, reagents and it was proved to be rugged. The developed normal phase chiral LC method can be used
for the determination of the enantiomeric purity of R-β-amino-β-(4-methoxyphenyl) propionic acid. |
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Keywords: | Column liquid chromatography Enantiomeric purity Validation and quantification Amino propionic acid |
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