comprehensive chemoselective and enantioselective 2D-HPLC set-up for fast enantiomer analysis of a multicomponent mixture of derivatized amino acids

A feasibility study on the fast enantioselective two-dimensional HPLC separation of racemic amino acid derivatives is presented. The method involves the on-line coupling of a narrow-bore C18 RP column in the first dimension to a short enantioselective column based on nonporous 1.5 μm particles modif...

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Bibliographic Details
Published in:Analytical and bioanalytical chemistry 2007-08, Vol.388 (8), p.1717-1724
Main Authors: Welsch, T, Schmidtkunz, C, Müller, B, Meier, F, Chlup, M, Köhne, A, Lämmerhofer, M, Lindner, W
Format: Article
Language:English
Subjects:
3,5-Dinitrobenzoyl amino acids
Amino Acids - isolation & purification
Chiral stationary phase
Chromatography, High Pressure Liquid - instrumentation
Chromatography, High Pressure Liquid - methods
Comprehensive two-dimensional high-performance liquid chromatography
Dinitrobenzenes
Enantioselective separation
Equipment Design
Feasibility Studies
Nonporous silica
O-9-(tert-butylcarbamoyl) quinidine
Reversed phase separation
Stereoisomerism
Sub-2-μm particles
Time Factors
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Summary:A feasibility study on the fast enantioselective two-dimensional HPLC separation of racemic amino acid derivatives is presented. The method involves the on-line coupling of a narrow-bore C18 RP column in the first dimension to a short enantioselective column based on nonporous 1.5 μm particles modified with quinidine carbamate as chiral selector in the second dimension. Conceptually, the system was designed to enable both time-controlled repeated transfer of fractions of the eluate and detector-controlled transfer of selected fractions from column 1 to column 2. To avoid volume overloading of the second chiral column, a narrow-bore reversed phase column was installed in the first dimension. Due to the fast (less than 1.5 minutes) enantiomer separation that occurs in the second dimension, the overall analysis time for the two-dimensional separation of a mixture of nine racemic 3,5-dinitrobenzoyl amino acids was optimized at 16 minutes.
ISSN:1618-2642
1618-2650
DOI:10.1007/s00216-007-1399-4