LC-MS/MS를 이용한 농산물중 Neonicotinoid 계 농약분석

• Published in: Han'gug sigpum wi'saeng anjeonseong haghoeji Vol. 35; no. 4; pp. 312 - 318
• Main Authors: 황래홍, 양혜란, 이재규, 김창규, 김민정, Hwang, Lae-hong, Yang, Hye-ran, Lee, Jae-kyoo, Kim, Chang-kyu, Kim, Min-jung
• Format: Journal Article
• Language: Korean
• Published: 한국식품위생안전성학회 31.08.2020
• Subjects: 식품과학; Neonicotinoid Pesticide; Agricultural product; LC-MS/MS
• ISSN: 1229-1153; 2465-9223
• DOI: 10.13103/JFHS.2020.35.4.312

A method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for neonicotinoid pesticide analysis in agricultural products. Four compounds (imidacloprid, clothianidin, acetamiprid, thiacloprid) were extracted with acetonitrile from agricultural products and cleaned up by NH2 solid-phase extraction procedure, and eluted with 0.1% formic acid in methanol/dichloromethane (5/95, v/v). The limit of detection and quantification were 0.0001-0.0005 mg/kg and 0.001 mg/kg, respectively. The mean recoveries of neonicotinoid pesticide from agricultural products were in the range of 90.7-100.9% and 94.4-99.8%, as spiked at 0.2 mg/kg and 0.02 mg/kg, respectively. This validation satisfied the national criteria for pesticide analytical methods. In summary, The present method is fast, precise and sensitive enough for the Positive List System (PLS), and we conclude that the method is also suitable for neonicotinoid pesticide determination in a wide range of agricultural products. LC-MS/MS를 이용하여 네오니코티노이드계 농약을 분석하는 방법을 연구하였다. 농산물 중 네오니코티노이드계 농약은 acetonitrile로 추출한 후 NH2 SPE cartridge을 이용하여 전처리를 수행하였으며, 용출액은 0.1% formic acid를 함유한 메탄올/디클로로메탄 혼합액(5/95, v/v)를 사용하였다. 4종의 네오니코티노이드계 농약(imidacloprid, clothianidin, acetamiprid, thiacloprid)의 최소 검출한계 및 정량한계는 경우 각각 0.0001-0.0005 mg/kg 및 0.001 mg/kg 이었다. 농산물에 각각 0.2 mg/kg 및 0.02 mg/kg 농도의 네오니코티노이드계 농약 4종을 첨가하여 분석 시 회수율은 각각 90.7-100.9%, 94.4-99.8% 범위였다. 본 시험법은 신속하고 정밀한 분석법으로 농약 허용물질목록제도(Positive List System (PLS))제도 적용에 필요한 충분한 검출감도를 나타내어 유통농산물에 대한 네오니코티노이드계 농약 분석에 적합한 것으로 조사되었다.