CCQM-K126: low polarity organic in water: carbamazepine in surface water

Abstract

The key comparison CCQM-K126 low polarity organic in water: carbamazepine in surface water was coordinated by Government Laboratory Hong Kong under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM).Eight National Metrology institutes or Designated Institutes participated and participants were requested to report the mass fraction of carbamazepine in surface water study material. The surface water sample was collected in Hong Kong and was gravimetrically spiked with standard solution. This study provided the means for assessing measurement capabilities for determination of low molecular weight analytes (mass range 100-500) and low polarity (pKOW ⩽ −2) in aqueous matrix. Nine NMIs/DIs registered for the KC and one withdrew before results were submitted. Nine results were submitted by the eight participants. Eight results applied the LC-MS/MS method and Isotope Dilution Mass Spectrometry approach for quantification. BAM additionally submitted a result from ELISA that was not included in the key comparison reference values (KCRV) calculation as is provided in the report for information. One further result was not included as the participant withdrew their result from the calculation after further analysis. The assigned KCRV was the median of the seven results and was assigned a KCRV of 250.2 ng/kg with a combined standard uncertainty of 3.6 ng/kg, The k-factor for the estimation of the expanded uncertainty of the KCRVs was chosen as k = 2.The degree of equivalence (with the KCRV) and its uncertainty was calculated for each result. Seven of the participants were able to demonstrate the ability to quantitatively determine low-polarity analyte in aqueous matrix by applying LC-MS/MS technique at a very low level.Main textTo reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/.The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).