NDLI: Indirect Enantioseparation of Amino Acids by CE Using Automated In-Capillary Derivatization with ortho-Phthalaldehyde and N-Acetyl-l-Cysteine

Content Provider	Springer Nature Link
Author	Kühnreich, Raphael Holzgrabe, Ulrike
Copyright Year	2016
Abstract	A simple CE method for the assessment of enantiomeric purity of individual amino acids (AAs) is presented. The AAs were derivatized with ortho-phthalaldehyde and a thiol in the capillary by means of successive hydrodynamic injections (5 s, 0.5 psi) of derivatization solution, sample and derivatization solution. A voltage of 1 kV was applied to blend the solutions and to start the reaction. Subsequently, the derivatives were separated using a background electrolyte (BGE) composed of 50 mM borate buffer (pH = 9.25) and 7.5 mM of a cyclodextrin (CD). To find the optimal derivatization reagent and CD, the impact of the thiols 3-mercaptopropionic acid (MPA), N-acetyl-l-cysteine (NAC) and N-isobutyryl-l-cysteine (NIBLC), and various neutral and negatively charged CDs on the resolution were assessed. The use of NAC and γ-CD enabled the best indirect enantioseparation of 16 AAs. Serine could be separated with β-CD, and proline and cysteine are not suitable for automated OPA-derivatization. The resolutions were ranging from 2.3 to 16.6. A method was validated representative for the AAs methionine, aspartic acid, tryptophan and phenylalanine. The recovery (n = 3) of the minor enantiomers was found to be within 95.1 and 107.5 %. The relative standard deviation (RSD) was ranging from 1.2 to 6.4 %. The method is accurate, precise, linear, and robust. For methionine it could be demonstrated that the ratio of l- and d-AA ranging from 1 to 99 % can be evaluated by direct comparison of the corrected peak areas with satisfactory accuracy ranging between 92.1 and 115.9 %.
Starting Page	1013
Ending Page	1022
Page Count	10
File Format	PDF
ISSN	00095893
Journal	Chromatographia
Volume Number	79
Issue Number	15-16
e-ISSN	16121112
Language	English
Publisher	Springer Berlin Heidelberg
Publisher Date	2016-06-17
Publisher Place	Berlin, Heidelberg
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Capillary electrophoresis Indirect enantioseparation Amino acids OPA derivatization Cyclodextrins Enantiomeric purity Chromatography Proteomics Pharmacy Laboratory Medicine
Content Type	Text
Resource Type	Article
Subject	Organic Chemistry Analytical Chemistry Biochemistry Clinical Biochemistry

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