High-performance liquid chromatography with mass spectrometry detection for quantitating COL-3, a chemically modified tetracycline, in human plasma

Michelle A. Rudek, Clark L. March, Kenneth S. Bauer, James M. Pluda, William D. Figg

Research output: Contribution to journalArticlepeer-review

Abstract

COL-3, 6-deoxy-6-demethyl-4-dedimethylamino-tetracycline, is a matrix metalloproteinase inhibitor. A specific and sensitive analytical method was necessary to quantitate the analyte in human plasma. High-performance liquid chromatography with atmospheric pressure chemical ionization mass spectrometry detection was utilized to quantitate COL-3 from 30 to 10 000 ng/ml in two calibration curves: 30-1500 and 400-10000 ng/ml. The sample preparation consisted of acetonitrile precipitation for all plasma samples. COL-3 is separated on a Waters Symmetry® C-18 (2.1 x 150 mm) column with oxalic acid (0.01 M, pH 2.2)-acetonitrile mobile phase. The total run time was 23 min. Identification of COL-3 and the internal standard was through positive chemical ionization and selective ion monitoring. A quantifying and qualifying ion for COL-3 is used to verify the presence of COL-3 in patient samples. Inter- and intra-run mean percent errors for all of the quality controls were less than 18.3% and relative standard deviations were all less than 14.9%. Recovery of COL-3 and the internal standard was approximately 55 and 72%, respectively. Freeze-thaw stability of COL-3 was variable. This method is suitable for quantifying COL-3 in patient samples and to further characterize the clinical pharmacology of this compound. (C) 2000 Elsevier Science B.V.

Original languageEnglish (US)
Pages (from-to)1003-1014
Number of pages12
JournalJournal of Pharmaceutical and Biomedical Analysis
Volume22
Issue number6
DOIs
StatePublished - Jul 2000
Externally publishedYes

Keywords

  • COL-3
  • Chromatography
  • Mass spectrometry
  • Tetracycline

ASJC Scopus subject areas

  • Analytical Chemistry
  • Pharmaceutical Science
  • Drug Discovery
  • Spectroscopy
  • Clinical Biochemistry

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