Clinical validation of a liquid chromatography single quadrupole mass spectrometry (LC-MS) method using Waters Kairos™ Amino Acid Kit reagents

Clin Chem Lab Med. 2025 Aug 8;63(11):2226-2235. doi: 10.1515/cclm-2025-0424. Print 2025 Oct 27.

Abstract

Objectives: Quantitation of plasma amino acids (AA) is critical for the diagnosis and monitoring of inherited disorders of AA metabolism. AA analysis using ion-exchange chromatography (IEC) with post-column ninhydrin derivatization is time consuming, with run times of ∼2 h, limiting sample throughput. Liquid chromatography mass-spectrometry can potentially address some of the current challenges.

Methods: Performance of components of the Waters Kairos Amino Acid Kit using liquid chromatography single quadrupole mass-spectrometry (LC-MS) following derivatization of samples with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AccQ•Tag™ Ultra Derivatization Reagent) was evaluated. Results were compared with the Biochrom-IEC method using patient specimens (n=115), ClinChek® control and external quality assessment (EQA) material.

Results: The kit reagents and our developed method had a 19-min analysis time, demonstrated acceptable inter-assay imprecision (CV<10 %) and bias vs. IEC-method (overall mean bias <2 %). Excellent correlation (concordance correlation coefficient (CCC) >0.99) with IEC was demonstrated for 10/23 analytes, good correlation (CCC >0.95) for 10/23, with the remaining three amino acids (aspartate, histidine and tryptophan) demonstrating moderate concordance (CCC ≥0.90 but <0.95). 1/23 AAs had a mean bias >10 % using EQA material. The method demonstrated a lower limit of quantitation of ≤2.5 μmol/L for all AA, making this assay suitable for CSF analysis. Calibration stability bias was <5 % over 12-weeks. Derivatized AAs were stable for ≤17 days. The analytical column supplied demonstrated good retention time stability (<0.4 %) and was capable of >2000 injections.

Conclusions: The tested methodology demonstrated good analytical performance and correlation with IEC. This approach confers practical advantages over IEC, including analytical selectivity and workflow time efficiency.

Keywords: amino acids; derivatization; liquid chromatography; mass spectrometry.

Publication types

  • Validation Study

MeSH terms

  • Amino Acids* / blood
  • Aminoquinolines
  • Carbamates / chemistry
  • Chromatography, Ion Exchange
  • Chromatography, Liquid / methods
  • Humans
  • Indicators and Reagents / chemistry
  • Liquid Chromatography-Mass Spectrometry
  • Mass Spectrometry* / methods
  • Reagent Kits, Diagnostic*

Substances

  • Amino Acids
  • Reagent Kits, Diagnostic
  • 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate
  • Indicators and Reagents
  • Carbamates
  • Aminoquinolines