Quantification of darunavir and etravirine in human peripheral blood mononuclear cells using high performance liquid chromatography tandem mass spectrometry (LC-MS/MS), clinical application in a cohort of 110 HIV-1 infected patients and evidence of a potential drug-drug interaction

Clin Biochem. 2016 May;49(7-8):580-6. doi: 10.1016/j.clinbiochem.2015.12.011. Epub 2015 Dec 29.

Abstract

Objectives: To describe the validation of a sensitive high performance liquid chromatography tandem mass spectrometry (LC-MS/MS) method allowing the simultaneous quantification of darunavir (DRV) and etravirine (ETR) in peripheral blood mononuclear cells (PBMCs) and its application in a cohort of HIV-1 infected patients.

Methods: Blood samples were obtained from 110 patients. PMBCs were isolated using density gradient centrifugation. Drug extraction from PBMCs was performed with a 60:40 methanol-water (MeOH-H2O) solution containing deuterated IS (DRV-d9 and ETR-d8). The chromatographic separation was performed on a RP18 XBridge™ column.

Results: The geometric mean (GM) of cell associated concentration ([DRV]CC) and plasmatic concentration ([DRV]plasma) were 360.5ng/mL (CI95%:294.5-441.2) and 1733ng/mL (CI95%:1486-2021), respectively. A geometric mean intracellular (IC)/plasma ratio (GMR) of 0.21 (CI95%:0.18-0.24) was calculated. Adjusted for dose/body surface area and post-intake time, a statistically significant correlation was observed between [DRV]Plasma and the eGFR (p=0.002) and between [DRV]Plasma and the concomitant use of ETR (p=0.038). For the 10 patients receiving ETR in addition to DRV, the GM of [ETR]Plasma (available for 8 out of 10 patients) and [ETR]CC were 492.3ng/mL and 2951ng/mL respectively. The GMR of ETR was 7.6 (CI95%: 3.61-13.83).

Conclusions: A handy and sensitive high performance LC-MS/MS method allowing the simultaneous quantification of DRV and ETR in PBMCs has been described and successfully applied in the largest cohort of DRV-treated patients reported to date. ETR accumulates more efficiently in PBMCs compared to DRV. We have also highlighted a possible impact of ETR on DRV plasma concentrations requiring further investigations.

Keywords: Anti-retroviral drugs; Darunavir; Drug interaction; Etravirine; HIV-1; Intracellular; LC–MS/MS; PBMCs.

MeSH terms

  • Biomarkers / metabolism*
  • Chromatography, High Pressure Liquid / methods*
  • Cohort Studies
  • Darunavir / blood*
  • Darunavir / therapeutic use
  • Drug Interactions
  • Drug Monitoring / methods
  • Female
  • Follow-Up Studies
  • HIV / drug effects
  • HIV Infections / blood*
  • HIV Infections / drug therapy
  • HIV Protease Inhibitors / blood
  • HIV Protease Inhibitors / therapeutic use
  • Humans
  • Leukocytes, Mononuclear / drug effects
  • Leukocytes, Mononuclear / metabolism*
  • Limit of Detection
  • Male
  • Middle Aged
  • Nitriles
  • Prognosis
  • Pyridazines / blood*
  • Pyridazines / therapeutic use
  • Pyrimidines
  • Reverse Transcriptase Inhibitors / blood
  • Reverse Transcriptase Inhibitors / therapeutic use
  • Tandem Mass Spectrometry / methods*

Substances

  • Biomarkers
  • HIV Protease Inhibitors
  • Nitriles
  • Pyridazines
  • Pyrimidines
  • Reverse Transcriptase Inhibitors
  • etravirine
  • Darunavir