ISSN:
1052-9306
Keywords:
Chemistry
;
Analytical Chemistry and Spectroscopy
Source:
Wiley InterScience Backfile Collection 1832-2000
Topics:
Chemistry and Pharmacology
Notes:
An analytical method has been developed and validated for the quantitative determination of the N-methyl-D-aspartate (NMDA) antagonist cis-4-phosphonomethyl-2-piperidine carboxylic acid (CGS 19755) in human plasma. It is a member of a new class of compounds with the potential to be neuroprotective and attenuate neuronal damage resulting from brain trauma caused by stroke and head trauma. The method is based on gas chromatography/mass spectrometry and uses stable-isotope labeled CGS 19755 as the internal standard. Samples (1 ml) were first acidified (pH 2), then extracted using a solid-phase aminopropyl ion exchange column. The drug was eluted with NH4OH and evaporated until dry. Extracts were derivatized with a mixture of pentafluoropropionic anhydride and pentafluoropropanol, and analyzed by gas chromatography/mass spectrometry. Separation was accomplished on a DB-225 capillary column (15 m × 0.32 mm) with a 0.25 μ film thickness. Mass spectrometry was carried out under negative ion ammonia chemical ionization conditions with selected ion monitoring at m/z 760 and 764 for derivatized CGS 19755 and the internal standard, respectively. Specificity was shown by the lack of interfering peaks at the retention time of CGS 19755 and internal standard. Recovery and reproducibility assessments show good accuracy, precision and linearity over the validated concentration range of 2-5000 ng ml-1.
Additional Material:
4 Ill.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1002/bms.1200230905
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