Determination of cortisol production rates with contemporary liquid chromatography-mass spectrometry to measure cortisol-d(3) dilution after infusion of deuterated tracer

Clin Biochem. 2011 Apr;44(5-6):430-4. doi: 10.1016/j.clinbiochem.2010.12.008. Epub 2010 Dec 23.

Abstract

Objectives: Measurement of 24-h cortisol production rate (CPR) using steady-state infusion of deuterated cortisol and analysis of stable-isotope dilution by MS is a valuable tool to examine hypothalamic-pituitary-adrenal axis activity in humans. We have developed and validated an improved method for measuring cortisol dilution with contemporary LC-MS technology.

Design and methods: Plasma samples and calibrators were extracted with ethylacetate. LC-MS was performed with a Surveyor HPLC and TSQ Quantum triple-quadrupole mass spectrometer equipped with an atmospheric pressure chemical ionization (APCI) source.

Results: Selectivity was improved over previous methods via elimination of an interferent identified as 20β-dihydrocortisol. The LLOQ for cortisol-d(3) was 2.73nmol/L and LOD 1.37nmol/L. Plasma calibrators were linear over the concentration range 1.5-10% cortisol-d(3), with correlation coefficients >0.995.

Conclusions: This APCI LC-MS method offers simplified sample work-up and analysis and enables selective detection of the low concentration of cortisol-d(3) infused for determination of 24-h CPR.

Publication types

  • Research Support, N.I.H., Extramural
  • Validation Study

MeSH terms

  • Calibration
  • Chromatography, High Pressure Liquid / methods*
  • Deuterium
  • Humans
  • Hydrocortisone / biosynthesis*
  • Limit of Detection
  • Mass Spectrometry / methods*

Substances

  • Deuterium
  • Hydrocortisone