Highly sensitive determination of saquinavir in biological samples using liquid chromatography-tandem mass spectrometry

J Chromatogr B Analyt Technol Biomed Life Sci. 2003 Feb 5;784(2):233-42. doi: 10.1016/s1570-0232(02)00803-6.

Abstract

A selective and sensitive method for the determination of the HIV protease inhibitor saquinavir in human plasma, saliva, and urine using liquid-liquid extraction and LC-MS-MS has been developed, validated, and applied to samples of a healthy individual. After extraction with ethyl acetate, sample extracts were chromatographed isocratically within 5 min on Kromasil RP-18. The drug was detected with tandem mass spectrometry in the selected reaction monitoring mode using an electrospray ion source and 2H(5)-saquinavir as internal standard. The limit of quantification was 0.05 ng/mL. The accuracy of the method varied between -1 and +10% (SD within-batch) and the precision ranged from +4 to +10% (SD batch-to-batch). The method is linear at least within 0.05 and 87.6 ng/mL. After a regular oral dose (600 mg) saquinavir concentrations were detectable for 48 h in plasma and were well correlated with saliva concentrations (r(2)=0.9348, mean saliva/plasma ratio 1:15.1). The method is well suited for low saquinavir concentrations in different matrices.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Chromatography, Liquid / methods*
  • HIV Protease Inhibitors / analysis*
  • HIV Protease Inhibitors / blood
  • HIV Protease Inhibitors / urine
  • Humans
  • Male
  • Mass Spectrometry / methods*
  • Reference Standards
  • Saliva / chemistry
  • Saquinavir / analysis*
  • Saquinavir / blood
  • Saquinavir / urine
  • Sensitivity and Specificity

Substances

  • HIV Protease Inhibitors
  • Saquinavir