Performance evaluation of the LC-MS/MS method for determination of chlorates in plant-origin foodstuffs

Srđan Stefanović; Čaba Silađi; Danka Spirić; Radivoj Petronijević; Aleksandar Bajčić; Nikola Betić; Vedrana Jelušić

doi:10.18485/meattech.2025.66.3.96

Srđan Stefanović Institute of Meat Hygiene and Technology, Belgrade, Serbia https://orcid.org/0000-0002-8011-5654
Čaba Silađi Institute of Meat Hygiene and Technology, Belgrade, Serbia https://orcid.org/0009-0004-1933-3849
Danka Spirić Institute of Meat Hygiene and Technology, Belgrade, Serbia https://orcid.org/0000-0002-6008-7625
Radivoj Petronijević Institute of Meat Hygiene and Technology, Belgrade, Serbia https://orcid.org/0000-0002-3901-3824
Aleksandar Bajčić Institute of Meat Hygiene and Technology, Belgrade, Serbia https://orcid.org/0000-0003-2923-4137
Nikola Betić Institute of Meat Hygiene and Technology, Belgrade, Serbia https://orcid.org/0000-0002-7375-6752
Vedrana Jelušić Veterinary Office of Bosnia and Herzegovina, Sarajevo, Bosnia and Herzegovina

DOI: https://doi.org/10.18485/meattech.2025.66.3.96

Keywords: Chlorate, LC-MS/MS, validation, SANTE, Hypercarb™

Abstract

Chlorate (ClO₃^-) is a monovalent inorganic anion obtained by deprotonation of chloric acid. Its widespread historic use (as an herbicide) and numerous present applications result in notable findings of chlorate residues in food commodities. The aim of this paper is to present validation data confirming the fitness for purpose of the modified “QuPPe” method for LC-MS/MS determination of chlorate in plant-origin foodstuffs with high water content. The validation study was conducted according to SANTE 11312/2021 in the form of a full initial validation on three matrices representative of the leafy vegetable group.

The results of the key validation parameters demonstrate the fitness for purpose of the proposed method. Recovery values (96.5-105.3%), repeatability (4.1-16.2%), intermediate precision (3.9-16.4%) and expanded measurement uncertainty (12.6-32.1%) are in compliance with the criteria laid down in the SANTE document. Use of a graphitized carbon column for the separation of chlorate introduces the necessary step of frequent preconditioning with planar compounds e.g., chlorophyll. However, this process does not result in significant delays or extended run times if carried out regularly.