Enantiomeric Separation of Docetaxel Starting Material by Chiral LC Using Amylose Based Stationary Phase
2009
Ravikumar, M. | Narasimhanaidu, M. | Srinivasulu, K. | Raju, T Satyanarayana | Reddy, M Raja Sekhar | Swamy, P Yadagiri
The present work narrates an LC method for determination of enantiomeric purity of (4S,5R)-3,5-oxazolidinedicarboxylic acid 2,2-dimethyl-4-phenyl-3-(1,1-dimethylethyl) ester, which is a key starting material of docetaxel, an antineoplastic agent and belongs to the taxoid family. Resolution between enantiomers was achieved ≥4.0 within 30 min on Chiralpak AD-H (250 mm × 4.6 mm) column using n-hexane, 2-propanol, ethanol and trifluoroacetic acid (97.5, 1.5, 1.0, 0.15 v/v) as mobile phase at a flow rate of 1.0 mL min⁻¹ at 25 °C. The detection was made at 215 nm using UV detection. The effects of 2-propanol, ethanol and temperature on enantioselectivity and resolution of enantiomers were evaluated. The method was validated for (4R,5S)-enantiomeric impurity in terms of accuracy, precision and linearity in the range of 0.5–5 μg mL⁻¹ and the correlation coefficient was >0.999. The recoveries were 93.2–104.4%. The limits of detection (LOD) and quantification (LOQ) of unwanted (4R,5S)-enantiomer was 0.1 and 0.5 μg mL⁻¹. The method was found to be suitable for rapid quantification of (4R,5S)-enantiomer of docetaxel starting material.
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