A normal phase HPLC chiral purity method with sample derivatization is described for a small molecule chiral compound with no UV chromophore. This method used a 5-dinitrobenzyol chloride as derivatization reagent with a selective base for the derivatization. The derivation was allowed to occur for 30 minutes, and the resulting sample solutions were further extracted and then analyzed by HPLC with UV detection. The HPLC method used Regis Technologies Inc. Kromasil (S,S)-Whelk-O1, 4.6 x 250 mm, 5mm column and 75/25 (v/v) Hexane/ Ethanol with 0.1% DEA as mobile phase. With the optimization of the conditions for derivation and HPLC, the method was shown to be specific, accurate, reproducible, and sensitive for the analysis of this chiral compound. A representative chromatogram for the chiral separation was shown. The method has been applied for the release testing of the starting material batches for GMP production.

Chiral method development for a small molecule starting material by derivatization and high pressure liquid chromatography

248th National Meeting (2014)

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