Validation of the QuEChERSER mega-method for the analysis of pesticides, veterinary drugs, and environmental contaminants in tilapia (Oreochromis Niloticus)

Authors: MONTEIRO, SERGIO - Biological Institute, Brazil; Lehotay, Steven; Sapozhnikova, Yelena; NINGA, EDERINA - Veterinary Institute; MOURA ANDRADE, GRAZIELA - Biological Institute, Brazil; Lightfield, Alan

Submitted to: Food Additives & Contaminants. Part A: Chemistry, Analysis, Control, Exposure & Risk Assessment
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 12/1/2021
Publication Date: 1/27/2022
Citation: Monteiro, S.H., Lehotay, S.J., Sapozhnikova, Y.V., Ninga, E., Moura Andrade, G.C., Lightfield, A.R. 2022. Validation of the QuEChERSER mega-method for the analysis of pesticides, veterinary drugs, and environmental contaminants in tilapia (Oreochromis Niloticus). Food Additives & Contaminants. Part A. 39:699-709. https://doi.org/10.1080/19440049.2021.2020911.
DOI: https://doi.org/10.1080/19440049.2021.2020911

Interpretive Summary: Aquaculture continues to grow worldwide to meet increased demand for fish consumption. Fast and efficient testing methods for analysis of many diverse chemical contaminants in fish are needed to comply with food safety regulations. In this study, we validated recently developed mega-method, QuEChERSER, more than QuEChERS (quick, easy, effective, rugged and safe) for the analysis of pesticides, veterinary drugs, and environmental contaminants in tilapia (Oreochromis Niloticus). The results demonstrated that the QuEChERSER mega-method can be implemented to expand analytical scope and increase laboratory efficiency compared to the QuEChERS method in any analytical testing laboratory.

Technical Abstract: Diverse food safety programs around the world are designed to help ensure production of safe food. To meet this need, the development and implementation of more efficient and effective analytical methods to monitor pesticides and other contaminants in foods is important. In this study, we report the validation results for a simple high-throughput mega-method for residual analysis of 213 pesticides and veterinary drugs, including 15 metabolites, plus 12 environmental contaminants (polychlorinated biphenyls) in tilapia muscle for implementation in routine laboratory analyses. The generic sample preparation method and analytical approach is known as QuEChERSER (more than QuEChERS). A small portion of the initial extract (200 µL) is taken for analysis by ultrahigh-performance liquid chromatography (UHPLC) tandem mass spectrometry (MS/MS) covering 145 analytes, and the remaining extract undergoes a salting out step followed by an automated robotic instrument top sample preparation (ITSP) cleanup, also known as micro-solid-phase extraction (µSPE), plus fast low-pressure gas chromatography LPGC-MS/MS for 134 analytes (66 pesticides are targeted in both UHPLC-MS/MS and LPGC-MS/MS). The mega-method was validated in spiked tilapia samples at 5, 10, 15, and 20 ng/g with 10 replicates per level over two days (n = 80 overall), and 70–140% recoveries with RSDs =20% were achieved for 92% of the analytes in LC and 82% in GC. No significant matrix effects were observed for the analytes in LPGC-MS/MS, and only 5% of the analytes exceeded ±20% matrix effect in UHPLC-MS/MS. Analysis of standard reference materials (NIST SRMs 1946 and 1947) for contaminants in freeze-dried fish showed acceptable results, further demonstrating that the QuEChERSER mega-method can be implemented to expand analytical scope and increase laboratory efficiency compared to the QuEChERS method.