Bifenthrin Residues in Table Grapevine: Method Optimization, Dissipation and Removal of Residues in Grapes and Grape Leaves

Abstract

The QuEChERS method was adjusted to determine bifenthrin residues in grapes and grape leaves. Extraction and cleanup procedures were optimized to decrease co-extracted materials and enhance the detection of bifenthrin. The method was validated per the European Union (EU) Guidelines criteria. Accuracy ranged from 98.8% to 93.5% for grapes and grape leaves, respectively. Precision values were 5.5 and 6.4 (RSDr) and 7.4 and 6.7 (RSD_R) for grapes and grape leaves, respectively. LOQs (the lowest spiking level) were 2 and 20 µg/kg for grapes and grape leaves, respectively. Linearity as determination coefficient (R²) values were 0.9997 and 0.9964 for grapes and grape leaves, respectively, in a matrix over 1-100 µg/L range of analyte concentration. This was very close to the value in the pure solvent (0.9999), showing the efficiency of the cleanup in removing the co-extracted and co-injected materials; the matrix effect was close to zero in both sample matrices. Dissipation of bifenthrin was studied in a supervised trial conducted in a grapevine field during the summer of 2023 at the recommended dose and double the dose. Dissipation factor k values were 0.1549 and 0.1672 (recommended dose) and 0.235 and 0.208 (double dose) for grapes and grape leaves, respectively. Pre-harvest interval (PHI) was calculated for the Maximum Residue Limit (MRL) values of the EU database. Residues of bifenthrin were removed effectively from grapes using simple washing with tap water in a laboratory study. Residues reached the MRL level of 0.3 mg/kg in both washing treatments, running or soaking in tap water treatments for 5 min. Removal from leaves did not decrease residue levels to the MRL in grape leaves.

Keywords: bifenthrin pesticide; dissipation; grapes; method validation; pesticide residues removal.

Figure 1

Full scan spectrum (a), optimized Rf Lens (b), breakdown curve at 1.5 mTorr (+) (c), and product spectrum (d) of bifenthrin.

Figure 2

(a) The efficiency of various adsorbents and dilution ratios in grape leaf extract cleanup at 0.1 mg/kg (n = 5). (b) Raw extract of grape leaves (1), 2x dil (2), 5x dil (3), 10x dil (4), PSA + C18 (5), PSA + C18 + 2.5 MWCNTs (6), PSA + C18 + 5 MWCNTs (7), PSA + C18 + 5x dil (8), PSA + C18 + 2.5 MWCNTs + 5x dil (9), and PSA + C18 + 5 MWCNTs + 5x dil (10).