Stable-labeled analogues and reliable quantification of nonprotein biomarkers by LC-MS/MS

Bioanalysis. 2010 Jan;2(1):69-80. doi: 10.4155/bio.09.166.

Abstract

Background: The aim was to develop, and establish as suitable to begin assessment by full validation, a quantitative LC-MS/MS method for asparagine in human plasma. Therein, to utilize a stable-labeled analogue of asparagine to act as surrogate analyte, producing complete calibration curves and corresponding QC samples and another m/z distinct stable-labeled analogue to act as internal standard.

Results: From two candidates, the surrogate analyte was selected through statistical comparisons of concentration-response data and the resultant method employed protein precipitation and LC on an unmodified silica column with multiple reaction monitoring detection mode. The calibration range was 50-10,000 ng/ml.

Conclusion: This method was successfully proven to meet the accuracy and precision acceptance criteria of current bioanalytical method validation guidelines.

MeSH terms

  • Asparagine / blood*
  • Biomarkers / blood
  • Chromatography, Liquid / methods*
  • Humans
  • Nitrogen Isotopes / blood*
  • Reproducibility of Results
  • Tandem Mass Spectrometry / methods*
  • Tandem Mass Spectrometry / standards

Substances

  • Biomarkers
  • Nitrogen Isotopes
  • Asparagine