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. 2023 Feb 23:17:100603.
doi: 10.1016/j.fochx.2023.100603. eCollection 2023 Mar 30.

Residue detection and correlation analysis of multiple neonicotinoid insecticides and their metabolites in edible herbs

Yudan Wang  1 , Jia'an Qin  1   2 , Qian Lu  1 , Jiao Tian  1 , Tongwei Ke  1 , Mengyue Guo  1 , Jiaoyang Luo  1 , Meihua Yang  1
Affiliations

Residue detection and correlation analysis of multiple neonicotinoid insecticides and their metabolites in edible herbs

Yudan Wang et al. Food Chem X. .

Abstract

In this work, a green analytical method was established for the simultaneous extraction and detection of 20 analytes-10 neonicotinoid insecticides and their 10 major toxic metabolites in edible herbs. QuEChERS and LC-MS/MS were used to analyze the 20 analytes in five edible herbs. The residues of the 20 neonicotinoid insecticides and their metabolites in 109 herbal samples were detected, of which 90 samples were positive, and the residue of total neonicotinoid insecticides ranged from 0.26 to 139.28 μg/kg. Acetamiprid (77.06 %, ≤85.95 μg/kg), imidacloprid (67.89 %, ≤32.49 μg/kg) and their metabolites (N-desmethyl-acetamiprid (44.04 %, ≤18.42 μg/kg) and desnitro imidacloprid (48.62 %, ≤16.55 μg/kg) were most frequently detected in herbs. Significant positive correlations were found between imidacloprid/acetamiprid and their metabolites in Lycii fructus and Citri reticulatae pericarpium. Therefore, more attention may be given to the neonicotinoid insecticide residues in edible herbs in the future.

Keywords: 1-methyl-3-(tetrahydro-3-furylmethyl) guanidium dihydrogen (PubChem CID: 16760148); 1-methyl-3-(tetrahydro-3-furylmethyl) urea (PubChem CID: 71346722); 4-trifluoromethylnicotinic acid (PubChem CID: 2777549); 5-hydroxy imidacloprid (PubChem CID: 137177224); 6-chloronicotinic acid (PubChem CID: 79222); Acetamiprid (PubChem CID: 213021); Clothianidin (PubChem CID: 86287519); Desnitro imidacloprid (PubChem CID: 274156523); Dinotefuran (PubChem CID: 100958102); Flonicamid (PubChem CID: 9834513); Flupyradifurone (PubChem CID: 16752772); Herbs; Hydroxy imidacloprid (PubChem CID: 125288315); IMI-olefin (PubChem CID: 14626249); IMI-urea (PubChem CID: 15390532); Imidacloprid (PubChem CID: 86287518); LC-MS/MS; N-desmethyl-acetamiprid (PubChem CID: 11344811); Neonicotinoid insecticides; Nitenpyram (PubChem CID: 3034287); Pesticide residues; QuEChERS; Sulfoxaflor (PubChem CID: 16723172); Thiacloprid (PubChem CID: 115224); Thiamethoxam (PubChem CID: 107646).

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Conflict of interest statement

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Figures

Fig. 1
Fig. 1
Optimization of UFLC-MS/MS conditions: (A) MRM chromatogram; (B) EPI spectra of OH-IMI and 5-OH-IMI; (C) mobile phase composition: 1) acetonitrile–water, 2) acetonitrile–water (5 mM ammonium formate), 3) acetonitrile–water (0.1 % formic acid), 4) acetonitrile–water (0.1 % formic acid and 5 mM ammonium formate).
Fig. 2
Fig. 2
Optimization of QuEChERS sample preparation (A) extraction solvent; (B) clean-up phase.
Fig. 3
Fig. 3
Recoveries of NEOs and m-NEOs at three different levels for five matrices (n = 5). (A) Low level; (B) medium level; (C) high level.
Fig. 4
Fig. 4
The residue concentrations and residue rates of NEOs and m-NEOs in positive samples: (A) residue concentrations; (B) residue rates.
Fig. 5
Fig. 5
Correlation analysis of NEOs and m-NEOs in (A) Lycii fructus and (B) Citri reticulatae pericarpium.
Fig. 5
Fig. 5
Correlation analysis of NEOs and m-NEOs in (A) Lycii fructus and (B) Citri reticulatae pericarpium.
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