Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry for Cyclosporine Analysis in Human Whole Blood and Comparison With an Antibody-Conjugated Magnetic Immunoassay

Ther Drug Monit. 2018 Feb;40(1):69-75. doi: 10.1097/FTD.0000000000000477.

Abstract

Background: Various immunoassays have been used for cyclosporine A (CsA) analysis in human whole blood; however, they could not fully satisfy the requirements of criteria for accuracy and specificity in CsA measurement. The liquid chromatography tandem mass spectrometry is a gold method for CsA analysis. The aim of the study was to develop and validate an ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for CsA analysis and establish its agreement with an antibody-conjugated magnetic immunoassay (ACMIA) in clinical sample analysis.

Methods: An UHPLC-MS/MS method for CsA analysis in human whole blood was developed, validated, and applied in 85 samples, which were also tested by ACMIA. The agreement between UHPLC-MS/MS and ACMIA was evaluated by Bland-Altman plot.

Results: The calibration range was 5-2000 ng/mL. The inaccuracy and imprecision were -4.60% to 5.56% and less than 8.57%, respectively. The internal standard-normalized recovery and matrix factor were 100.4%-110.5% and 93.5%-107.6%, respectively. The measurements of ACMIA and UHPLC-MS/MS were strongly correlated (r > 0.98). Evaluated by Bland-Altman plot, the 95% limit of agreement of the ACMIA:UHPLC-MS/MS ratio was 88.7%-165.6%, and the mean bias of the ratio was 21.1%.

Conclusions: A rapid, simple, accurate, and reliable UHPLC-MS/MS method for CsA analysis in human whole blood was developed, validated, and applied in 85 samples. On average, 21.1% overestimation was observed in ACMIA compared with that in the UHPLC-MS/MS. Further and larger studies are required to identify whether this degree of variance could be accepted by clinicians.

Publication types

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

MeSH terms

  • Chromatography, High Pressure Liquid / methods*
  • Cyclosporine / blood*
  • Drug Monitoring / methods
  • Humans
  • Immunoassay / methods*
  • Immunosuppressive Agents / blood
  • Magnetics
  • Tandem Mass Spectrometry / methods*

Substances

  • Immunosuppressive Agents
  • Cyclosporine