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Determination of stable isotopically substituted histidine in human plasma by gas chromatography-mass spectrometry

Authors
Journal
Journal of Chromatography B Biomedical Sciences and Applications
0378-4347
Publisher
Elsevier
Publication Date
Volume
413
Identifiers
DOI: 10.1016/0378-4347(87)80207-4
Disciplines
  • Pharmacology

Abstract

Abstract A gas chromatographic-election-impact mass spectrometric method for the determination of stable isotopically substituted histidine in human plasma has been developed. Histidine was derivatized to αN-trifluoroacetyl- imN-carbethoxyhistidine n-butyl ester 9TCB derivative) by a three-step reaction: an initial esterification by 3 M n-butanolic hydrochloric acid, followed by trifluoroacetylation with trifluoroacetic anhydride and then ethoxycarbonylation with diethyl pyrocarbonate. Quantitation was carried out by selected-ion monitoring on the molecular ions ( m/z 379,383 and 385) of the respective TCB derivatives of histidine, [1- 15N,5,ββ- 2H 3]histidine (histidine-[M+4]) and [1,3- 15N 2,5,α,ββ- 2H 4]histidine (histidine-[M+6]). The sensitivity, specificity, precision and accuracy of the method were demonstrated to be satisfactory for application to a pharmacokinetic study of histidine after administration of a trace amount of stable isotopically substituted histidine (histidine-[M+4]) in humans.

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