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신서영 ( Seoyoung Shin ),박인주 ( Inju Park ),이정미 ( Jung Mi Lee ),장귀현 ( Gui-hyun Jang ),김현경 ( Hyun-kyung Kim ),허수정 ( Soojung Hu ),남봉현 ( Bonghyeon Nam ) 한국환경농학회 2023 한국환경농학회 학술대회집 Vol.2023 No.0
Nereistoxin is a natural toxin found in lugworms. Bensultap, cartap, thiocyclam and thiosultap, which are insecticides derived from the molecular structure of nereistoxin, are rapidly converted into nereistoxin in vivo and in the environment after spraying the drug, which binds to nicotinic acetycholine receptor of insects. It shows an insecticidal activity by inhibition of the Na+ and K+ conduction at the end plate membrane, which causes paralysis of central nervous system of insects. In Korea, the definition of residues of bensultap, cartap and thiocyclam is managed as nereistoxin. Currently, the analytical method of nereistoxin residue has a complicated and time-consuming process. Therefore, we tried to improve the usability and efficiency with the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method so that it can be safely converted to nereistoxin. In this study, the validation for the quantitative analysis of nereistoxin was performed, which was verified by the Ministry of Food and Drug Safety. Five agricultural products (mandarin, potato, soybean, hulled rice, and chili pepper) showing group representatives were chosen for experiments. In order to extract, L-cysteine was added into the samples and mixed thoroughly. The samples were heated at 70℃ with 3% nickel chloride and 28% ammonium hydroxide to convert into the nereistoxin rapidly. After addition of sodium chloride and acetonitrile, centrifugation was performed followed by purification using dispersive solid-phase extraction (d-SPE) with anhydrous magnesium sulfate and primary and secondary amine (PSA) to remove the interferences in samples. The results of LC-MS/MS analysis using amide column show the linear standard calibration curves with r-square values higher than 0.99 (coefficient of determination with calibration range) and mean recovery rates of nereistoxin ranged at 84.4~106.2%, the precision less than 12.6% in all five samples. These results are suitable for CODEX guideline for residue analysis (CAC/GL 40). In summary, the proposed method for determination of nereistoxin residue in foods could be included in the Korean Food Code for enabling the safety management of pesticides.