State-of-the-art of serum testosterone measurement by isotope dilution-liquid chromatography-tandem mass spectrometry

Clin Chem. 2008 Aug;54(8):1290-7. doi: 10.1373/clinchem.2008.105841. Epub 2008 Jun 12.

Abstract

Background: The recent interest of clinical laboratories in developing serum testosterone assays based on isotope dilution-liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) stems from the lack of accuracy of direct immunoassays. In this study, we assessed the accuracy and state of standardization (traceability) of 4 published ID-LC-MS/MS procedures in a method comparison with an ID-gas chromatography (GC)-MS reference measurement procedure listed in the database of the Joint Committee for Traceability in Laboratory Medicine.

Methods: The study used 58 specimens from different patient categories. Each specimen was measured in triplicate (ID-LC-MS/MS) and quadruplicate (ID-GC-MS) in independent runs.

Results: The testosterone concentrations by ID-GC-MS were 0.2-4.4 nmol/L (women), 0.2-2.0 nmol/L (hypogonadal man), and 10.1-31.3 nmol/L (normogonadal men). For ID-GC-MS, the CV was nearly constant, with a median of 1.0%; for ID-LC-MS/MS, it was concentration-dependent, with a median of up to 8%. Weighted Deming regression gave mean slopes, intercepts, and correlation coefficients of 0.90-1.11, -0.055-0.013 nmol/L, and 0.993-0.997, respectively. The % difference plot showed between 7% and 26% of the results outside a total error limit of 14%, with median deviations from ID-GC-MS between -9.6 and 0.4%.

Conclusions: This study demonstrated fairly good accuracy and standardization of the tested ID-LC-MS/MS procedures. Performance differences between procedures were evident in some instances, due to improper calibration and between-run calibration control. This emphasizes the need for thorough validation, including traceability, of new ID-LC-MS/MS procedures.

Publication types

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

MeSH terms

  • Adolescent
  • Adult
  • Calibration
  • Carbon Isotopes
  • Chromatography, Liquid / methods*
  • Female
  • Humans
  • Hypogonadism / blood
  • Indicator Dilution Techniques
  • Male
  • Middle Aged
  • Reference Standards
  • Regression Analysis
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Specimen Handling
  • Tandem Mass Spectrometry / methods*
  • Testosterone / blood*

Substances

  • Carbon Isotopes
  • Testosterone