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Validation of an HPLC-MS/MS Method to Determine Pesticides Residues in Rice
* 1, 2 , 2 , 2, 3 , 1, 4 , 1, 2, 5, 6
1  University of Coimbra, Faculty of Pharmacy, Polo III, Azinhaga de St. Comba, 3000-548 Coimbra, Portugal
2  National Institute for Agrarian and Veterinary Research (INIAV), I.P., Av. da República 2780-157 Oeiras, Portugal
3  GREEN-IT Bioresources for Sustainability, ITQB NOVA, Av. da República, 2780-157 Oeiras, Portugal
4  REQUIMTE/LAVQ, R. D. Manuel II, Apartado 55142, Porto Portugal
5  Centre for Animal Science Studies (CECA), ICETA, University of Porto, 4501-401 Porto, Portugal
6  Associate Laboratory for Animal and Veterinary Sciences (Al4AnimalS), 1300-477 Lisbon, Portugal
Academic Editor: Qinchun Rao (registering DOI)

For a substantial portion of the global human population, rice is the most significant and primary cereal crop. 20% of the calories consumed globally come from rice, which is essential for the existence of more than 3.5 billion people (Shakoori et al., 2018). One of the most crucial aspects of growing grain production is the application of pesticides, including pre- and post-emergence herbicides, insecticides, and fungicides, at different phases of cultivation. However, the use of these pesticides has an impact on the soil and water. In addition to regularly used pesticides, a significant concern is the presence of not allowed pesticides in rice, which is why Good Manufacturing Practice (GMP) is crucial (Kresse et al., 2019; Shakoori et al., 2018). For this reason, there is an increasing interest in the development methodologies to detect pesticides residues in food and feed samples.

In the present study, a method was developed and validated to determine 121 pesticide residues in rice, according to the guidance document SANTE/11312/2021 (SANTE, 2021). QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) was chosen as the pesticide extraction method and the extract was analyzed by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The linear ranges of the calibration curves were between 5–100, 10–100 or 20-100 µg/L, depending on the pesticide. The limit of quantification was 5, 10, or 50 µg/kg. The methodology was shown to be precise and accurate (recovery 70.02 - 119.08%.) and was applied to commercial samples of rice.

Keywords: Rice; Pesticide residues; UHPLC-MS/MS