Assessment of the long-term stability of pesticide residues under freezing conditions in brown rice and soybean certified reference materials

The objective of this study was to assess the long-term stability of pesticide residues in brown rice and soybean. The long-term stability of pesticide residues in brown rice and soybean was assessed for 5415 days (over 14 years) and 1801 days (about 5 years), respectively. The samples-certified reference materials (CRMs) 7504-a (brown rice) and 7509-a (soybean) -were prepared by freeze-pulverization. Two target pesticides (etofenprox and fenitrothion) were selected for brown rice and four (chlorpyrifos, diazinon, fenitrothion, and permethrin) for soybean. Our analytical results for long-term stability based on highly reliable isotope dilution mass spectrometry were in the range of expanded uncertainty (k=2) for the certified values of each CRM. The concentration showed a decreasing trend in none of the target pesticides when the samples were stored at temperatures between -20 °C and -30 °C, which indicated that the target pesticides were stable for the tested long terms.