Validation and implementation of a method for determination of bryostatin 1 in human plasma by using liquid chromatography/tandem mass spectrometry

Ming Zhao, Michelle A. Rudek, Ping He, B. Douglas Smith, Sharyn D. Baker

Research output: Contribution to journalArticle

Abstract

A new sensitive and specific method using liquid chromatography/tandem mass spectrometry for determination of bryostatin 1 was developed and validated. Sample pretreatment involved a double liquid-liquid extraction step with a mixture of acetonitrile/n-butyl chloride (1/4, v/v). Separation of the compound of interest, including the internal standard paclitaxel, was achieved on a Waters X-Terra C18 (50 × 2.1 mm i.d., 3.5 μm) analytical column with acetonitrile/water mobile phase (80:20, v/v) containing 0.1% formic acid using isocratic flow at 0.15 mL/min for 13 min. The analytes of interest were monitored by tandem mass spectrometry with electrospray positive ionization. The linear calibration curves were generated over the range of 50-2000 pg/mL with values for the coefficient of determination of >0.99. The values for both within-day and between-day precision and accuracy were <15%. This method was used to characterize the plasma pharmacokinetics of bryostatin 1 at doses of 20 μg/m2 to optimize treatment with this agent.

Original languageEnglish (US)
Pages (from-to)143-148
Number of pages6
JournalAnalytical biochemistry
Volume337
Issue number1
DOIs
StatePublished - Feb 1 2005

Keywords

  • Bryostatin 1
  • LC/MS/MS
  • Pharmacokinetics

ASJC Scopus subject areas

  • Biophysics
  • Biochemistry
  • Molecular Biology
  • Cell Biology

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