Development and validation of an LC-MS-MS method for determination of methyl kulonate in rat plasma

Biomed Chromatogr. 2012 Jul;26(7):857-62. doi: 10.1002/bmc.1741.

Abstract

A sensitive, rapid and specific LC-MS-MS method was established and validated for determination of methyl kulonate, a major bioactive constituent isolated from Meliae Cortex, in rat plasma. Plasma samples were treated by precipitating protein with methanol and were chromatographed using a Capcell Pak C₁₈ column (100 x 4.6 mm, 5 μm) with the mobile phase comprising a mixture of methanol, 10 mM ammonium formate and formic acid (95:5:0.1, v/v/v). Detection and quantification were performed by mass spectrometry in the multiple reaction monitoring mode with positive atmospheric ionization at m/z 467 --> 311 for methyl kulonate, and m/z 469 --> 451 for dubione B (internal standard), respectively. A good linear response was observed over the concentration range 1.00-500 ng/mL with the lower limit of quantification 1.00 ng/mL in rat plasma. The method also afforded satisfactory results base on sensitivity, specificity, precision, accuracy, recovery, freeze-thaw and long-time stability. The validated method was successfully applied to determine the pharmacokinetic properties of methyl kulonate in rats after oral administration at dose of 100 mg/kg. This pharmacokinetic study of methyl kulonate is reported here for the first time.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Administration, Oral
  • Animals
  • Chromatography, Liquid / methods*
  • Chromatography, Liquid / standards
  • Drug Stability
  • Drugs, Chinese Herbal / administration & dosage
  • Drugs, Chinese Herbal / pharmacokinetics
  • Limonins / administration & dosage
  • Limonins / blood*
  • Limonins / pharmacokinetics
  • Linear Models
  • Male
  • Melia azedarach / chemistry
  • Rats
  • Rats, Sprague-Dawley
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Tandem Mass Spectrometry / methods*
  • Tandem Mass Spectrometry / standards

Substances

  • Drugs, Chinese Herbal
  • Limonins
  • methyl kulonate