Chiral separation and determination of excitatory amino acids in brain samples by CE-LIF using dual cyclodextrin system

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• 作者：Zsolt Wagner (1)
  Tamás Tábi (1)
  Tamás Jakó (1)
  Gergely Zachar (2)
  András Csillag (2)
  éva Sz?k? (1) eva.szoko@net.sote.hu
• 关键词：Chiral capillary electrophoresis – Neurotransmitter amino acids – d ; Aspartate – NBD ; F – Dual cyclodextrin system
• 刊名：Analytical and Bioanalytical Chemistry
• 出版年：2012
• 出版时间：November 2012
• 年：2012
• 卷：404
• 期：8
• 页码：2363-2368
• 全文大小：178.4 KB
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• 作者单位：1. Department of Pharmacodynamics, Semmelweis University, Nagyvárad tér 4, 1089 Budapest, Hungary2. Department of Anatomy, Histology and Embryology, Semmelweis University, T?zoltó u. 58, 1094 Budapest, Hungary
• ISSN：1618-2650

文摘

Chiral capillary electrophoresis method has been developed to separate aspartate and glutamate enantiomers to investigate the putative neuromodulator function of d-Asp in the central nervous system. To achieve appropriate detection sensitivity fluorescent derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiazole and laser-induced fluorescence detection was applied. Although, simultaneous baseline separation of the two enantiomer pairs could be achieved by using 3 mM 6-monodeoxy-6-mono(3-hydroxy)propylamino-β-cyclodextrin (HPA-β-CD), further improvement of the chemical selectivity was required because of the high excess of l-enantiomers in real samples to be analyzed. The system selectivity was fine-tuned by combination of 8 mM heptakis(2,6-di-O-methyl)-β-cyclodextrin and 5 mM HPA-β-CD in order to increase the resolution between aspartate and glutamate enantiomers. The method was validated for biological application. The limits of detection for d-Asp and d-Glu were 17 and 9 nM, respectively, while the limit of quantification for both analytes was 50 nM. This is the lowest quantification limit reported so far for NBD-tagged d-Asp and d-Glu obtained by validated capillary electrophoresis laser-induced fluorescence method. The applicability of the method was demonstrated by analyzing brain samples of 1-day-old chickens. In all the studied brain areas, the d-enantiomer contributed 1–2 % of the total aspartate content, corresponding to 17–45 nmol/g wet tissue.