Structural characterization of anti-HIV drug candidate PA-457 [3-O-(3',3'-dimethylsuccinyl)-betulinic acid] and its acyl glucuronides in rat bile and evaluation of in vitro stability in human and animal liver microsomes and plasma

Drug Metab Dispos. 2006 Sep;34(9):1436-42. doi: 10.1124/dmd.106.009233. Epub 2006 Jun 2.

Abstract

PA-457 [3-O-(3',3'-dimethylsuccinyl)-betulinic acid] represents a new class of anti-HIV drug candidates termed maturation inhibitors. After oral administration to rats, PA-457 was metabolized to several glucuronide conjugates and mainly eliminated into rat bile. Liquid chromatography-electrospray ionization-mass spectrometry analysis showed that the glucuronidation products of PA-457 were acyl glucuronides including one di-glucuronide, di-PA-457G, and two mono-glucuronides, referred to as mono-PA-457G (I) and mono-PA-457G (II), respectively. In-source fragmentation of MS spectra supported the conclusion that mono-PA-457G (I) was glucuronidated at the C-28 carboxyl of PA-457, whereas mono-PA-457G (II) was conjugated at the dimethylsuccinic acid side chain of the C-3 position. Quantification demonstrated that the predominant glucuronide of PA-457 in rat bile was mono-PA-457G (I) with lower amounts of mono-PA-457G (II) and di-PA-457G. In vitro stability indicated that the mono-acyl glucuronides of PA-457 were not degraded after incubation with 0.1 M phosphate buffer (pH 4, 7.4 and 9), plasma (human, rat, and mouse), and UDP-glucuronosyltransferase reaction media (without uridine 5'-diphosphoglucuronic acid) with microsomes (human, rat, and mouse liver microsomes), respectively, whereas the minor diglucuronide was unstable in rodent liver microsomes. All glucuronides of PA-457 could be hydrolyzed both by beta-glucuronidase and alkaline (1 M NaOH). Minor putative acyl migration products were slowly formed at pH 9, suggesting that the acyl glucuronides of PA-457 have relatively high in vitro stability.

Publication types

  • Research Support, N.I.H., Extramural
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Animals
  • Anti-HIV Agents / blood
  • Anti-HIV Agents / chemistry
  • Anti-HIV Agents / pharmacokinetics*
  • Bile / metabolism*
  • Biotransformation
  • Chromatography, Liquid / methods
  • Drug Stability
  • Glucuronides / chemistry
  • Glucuronides / metabolism*
  • Humans
  • Liver / metabolism
  • Male
  • Mice
  • Microsomes, Liver
  • Molecular Structure
  • Rats
  • Rats, Sprague-Dawley
  • Reproducibility of Results
  • Spectrometry, Mass, Electrospray Ionization / methods
  • Succinates / blood
  • Succinates / chemistry
  • Succinates / pharmacokinetics*
  • Triterpenes / blood
  • Triterpenes / chemistry
  • Triterpenes / pharmacokinetics*

Substances

  • Anti-HIV Agents
  • Glucuronides
  • Succinates
  • Triterpenes
  • bevirimat