Gas chromatography-isotope dilution mass spectrometry method validation for target pesticides in soybeans

The production of certified reference materials requires the application of highly accurate methods for characterisation. A gas chromatography-isotope dilution mass spectrometry method, setting ambitious performance criteria, was developed for eight selected pesticides in soybeans. Pressurised liquid extraction was followed by automated gel-permeation chromatography and solid-phase extraction clean-up. Pesticides identification respected a Commission Decision and guidelines of the Directorate General for Health and Food Safety (DG SANTE). Reliable quantification involved stable isotopically labelled analogues as internal standards. Validation, according to ISO/IEC 17,025 and DG SANTE guidelines, assessed linearity, LOD/LOQ, trueness, selectivity, precision, stability and robustness. Mean recoveries ranges (83–109%, relative standard deviations < 3%), repeatability (2.2–4.8%), day-to-day variation (0.6–4.2%) and combined uncertainty (1.2–4.2%) were fit for purpose. The method is highly accurate and suitable for certification of the selected pesticides in soybean matrix reference material.

HUERTAS-PEREZ Jose;  SEJEROE-OLSEN Berit;  GOKCEN Taner;  SANDOR F.;  SCHIMMEL Heinz;  DABRIO RAMOS Marta; 

2019-07-11

TAYLOR & FRANCIS LTD

JRC103539

1944-0049 (online),   

https://publications.jrc.ec.europa.eu/repository/handle/JRC103539,   

10.1080/19440049.2018.1538571 (online),