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Chiral separation of intact amino acids by capillary electrophoresis-mass spectrometry employing a partial filling technique with a crown ether carboxylic acid

Title
Chiral separation of intact amino acids by capillary electrophoresis-mass spectrometry employing a partial filling technique with a crown ether carboxylic acid
Authors
Lee S.Kim S.-J.Bang E.Na Y.-C.
Ewha Authors
나윤철
Issue Date
2019
Journal Title
Journal of Chromatography A
ISSN
0021-9673JCR Link
Citation
Journal of Chromatography A vol. 1586, pp. 128 - 138
Keywords
Carboxylic crown etherCE-MSChiral separationIntact amino acidsPartial filling separation
Publisher
Elsevier B.V.
Indexed
SCI; SCIE; SCOPUS scopus
Document Type
Article
Abstract
An enantiomeric separation method for underivatized free amino acids (AAs) using a partial filling technique with CE-MS was developed for the determination of D-AAs in vinegars. A typical chiral separation method was performed with different concentrations of (18-crown-6)-2,3,11,12-tetracarboxylic acid (18C6H4) dissolved in water or formic acid as the background electrolyte. Seventeen AAs, excluding proline and asparagine, were separated, showing chiral resolution values (Rs) ranging from 0.5 to 21.0. These results included baseline separations of 11 AAs, the peaks of which were observed as the ions [AA+18C6H4+H] + . The migration order of the chiral AAs was also evaluated, and the L-AAs migrated faster than the counterpart D-AAs except for serine, threonine and methionine when using (+)-18C6H4. To reduce contamination of the ESI source by the nonvolatile chiral selector and improve the ionization efficiency in partial filling technique, the separation zone length was adjusted to 70% of the capillary, which was filled with 30 mM 18C6H4 in water. This method showed a similar separation efficiency as the typical method, and the separated AA peaks were observed as free AA ions, [AA+H] + . The optimized method provided limits of detection (LODs) ranging from 0.07 to 1.03 μg/mL and good linearity (R 2 > 0.99) up to 50 μg/mL for DL-AAs. The developed method was utilized to determine DL-AAs in vinegars with a simple pretreatment process. It may be extended to sensitive AA analysis in the determination of minor enantiomeric impurities in the major component. © 2018 Elsevier B.V.
DOI
10.1016/j.chroma.2018.12.001
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자연과학대학 > 화학·나노과학전공 > Journal papers
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