These tools will no longer be maintained as of December 31, 2024. Archived website can be found here. PubMed4Hh GitHub repository can be found here. Contact NLM Customer Service if you have questions.


Pubmed for Handhelds

PUBMED FOR HANDHELDS

Search MEDLINE/PubMed

  • Title: Enantiomeric separation of TAPP, H-Tyr-(D)Ala-Phe-Phe-NH(2), by capillary electrophoresis using 18-crown-6-tetracarboxylic acid as a chiral selector.
    Author: Brunnkvist H, Karlberg B, Granelli I.
    Journal: J Chromatogr B Analyt Technol Biomed Life Sci; 2003 Aug 15; 793(2):343-50. PubMed ID: 12906909.
    Abstract:
    A capillary electrophoresis method for the enantiomeric separation of the tetrapeptide H-Tyr-(D)Ala-Phe-Phe-NH(2) (TAPP), has been developed and validated. The preferred background electrolyte (BGE) consisted of 0.1 M aqueous phosphoric acid adjusted to pH 3.0 with triethanolamine. The chiral selectors 18-crown-6-tetracarboxylic acid (18C6H(4)) and heptakis(2,6-di-O-methyl)-beta-cyclodextrin (2,6-DM-beta-CD) were compared and the crown ether 18C6H(4) was found to be superior. The separation of TAPP and its enantiomer was accomplished within 30 min with a resolution greater than 3.5. The method was then investigated with respect to selectivity, linearity, accuracy, range, precision, detection limit (DL), quantitation limit (QL) and robustness, essentially following International Conference of Harmonisation (ICH) guidelines for the validation of analytical methods. The DL and QL for the TAPP enantiomer were found to be 0.3 and 0.8%, respectively, at the target TAPP concentration of 1 mg/ml. Robustness was tested using a full factorial design for the following four experimental variables varied at two levels: pH of the BGE, chiral selector concentration in the BGE, phosphoric acid concentration in the BGE, and temperature. The method showed good performance with respect to all of the validation parameters, and proved to be robust to changes in the experimental parameters within the tested domain.
    [Abstract] [Full Text] [Related] [New Search]