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Stereoselective high-performance liquid chromatography and analytical method characterization of evacetrapib using a brush-type chiral stationary phase: A challenging isomeric separation requiring a unique eluent system.

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Title: Stereoselective high-performance liquid chromatography and analytical method characterization of evacetrapib using a brush-type chiral stationary phase: A challenging isomeric separation requiring a unique eluent system.
Authors: Sharp, V. Scott1 vss@lilly.com, Stafford, John D.2, Forbes, Robert A.2, Gokey, Megan A.1, Cooper, Mary R.1
Source: Journal of Chromatography A. Oct2014, Vol. 1363, p183-190. 8p.
Subjects: Stereoselective reactions, High performance liquid chromatography, Chiral stationary phases, Separation of enantiomers, Cardiovascular agents, Drug use testing, Drug analysis
Abstract: Using HPLC chiral separation screening, various columns representing the polysaccharide, macrocyclic antibiotic and brush classes were assessed in multiple chromatographic modes for the separation of evacetrapib, a potential cardiovascular drug, from its enantiomer, two diastereomers and several impurities. Screening data consistently pointed to the brush-type Whelk-O 1 chiral column as most promising for this task. A systematic separation optimization process is outlined using the ( S , S ) Whelk-O 1 chiral column, first for the resolution of the isomers, and later including six potential impurities. A relatively complex yet rugged separation system was eventually identified that effectively resolves all compounds within a reasonable analysis time, and should serve as an adequate tool for evacetrapib bulk drug enantiopurity measurement. [ABSTRACT FROM AUTHOR]
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Database: Engineering Source
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Abstract:Using HPLC chiral separation screening, various columns representing the polysaccharide, macrocyclic antibiotic and brush classes were assessed in multiple chromatographic modes for the separation of evacetrapib, a potential cardiovascular drug, from its enantiomer, two diastereomers and several impurities. Screening data consistently pointed to the brush-type Whelk-O 1 chiral column as most promising for this task. A systematic separation optimization process is outlined using the ( S , S ) Whelk-O 1 chiral column, first for the resolution of the isomers, and later including six potential impurities. A relatively complex yet rugged separation system was eventually identified that effectively resolves all compounds within a reasonable analysis time, and should serve as an adequate tool for evacetrapib bulk drug enantiopurity measurement. [ABSTRACT FROM AUTHOR]
ISSN:00219673
DOI:10.1016/j.chroma.2014.03.048