Gas-Liquid Chromatography를 이용한 사과 및 배 중의 농약 다성분 잔류분석법
Analysis of Multiple Pesticide in Apples and Pears using Gas-Liquid Chromatography
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사과 및 배 시료에서 농약 다성분의 gas chromatography를 이용한 잔류분석법 확립을 위하여 199가지의 농약을 선정하여 retention time 및 검출기에 따라 ECD 5 그룹 및 NPD 5 그룹의 10개 그룹으로 분류하였다. 시료의 종류에 따른 분석조건을 확립하기 위한 회수율 시험은 농약들의 log Pow 값과 화학적 분류에 따라 총 18개 (ECD 11개, NPD 7개)의 농약을 선정하였다. 예비실험 후 확립된 분석방법에 따라 10개 그룹의 혼합 표준용액으로 사과 및 배에 대한 회수율시험을 행하였다. 그 결과, 총 196가지의 농약의 70%에 해당하는 사과에서 136개, 배에서 133개의 농약들에서 회수율 70에서 120%의 양호한 결과를 나타내었다. 그러나 사과에서 43개, 배에서 45개의 농약들이 70% 미만의 회수율을 보였고, fenva- lerate는 120% 이상의 회수율을 나타내었으며, 사과에서 17개 및 배에서 18개의 농약들은 검출이 되지 않았다. 그러나 확립된 분석법은 SOP에 의한 신속하고 수월한 수행으로 농산물 중의 잔류농약을 검출 및 모니터링하는 목적에 적합하다고 사료된다.
Abstract
A rapid analytical method was developed to determine multiple pesticide residues in apples and pears using gas-liquid chromatography (GLC). The samples were extracted with water-miscible solvents and purified by cleanup procedures serially comprising liquid-liquid partition and solid-phase extraction (SPE). Each analyte was separated and determined by a high-resolution GLC equipped with electron-capture detector (ECD) and nitrogen-phosphorous detector (NPD). A total of 196 pesticides, which were previously classified into 5 groups each for ECD and NPD based on their retention behaviors on the capillary column and responses to the detector, were subjected to the recovery experiment. In compliance with the analytical criteria, 70 to 120% of recovery and less than 20% relative standard deviation, the proposed method could be successfully applied to analyze 136 and 133 pesticide residues in apples and pears, respectively, which enabled not only rapid screening but quantitation of the residues. Even though less reliability was resulted from unacceptable recovery range, rest of pesticides including 43 and 45 analytes in apples and pears, could be also detected for their identity. The proposed method, failed to cover 17 and 18 pesticides for apples and pears, which mostly showed high polarity or heat-lability but, could be suitable for fast surveilance or monitoring of fruit harvests.
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