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KMID : 0881720190340020115
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Journal of Food Hygiene and Safety
2019 Volume.34 No. 2 p.115 ~ p.123
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Development and Validation of an Analytical Method for Fenpropimorph in Agricultural Products Using QuEChERS and LC-MS/MS
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Lee Han-Sol
Do Jung-Ah
Park Ji-Su
Cho Sung-Min
Shin Hye-Sun
Jang Dong-Eun
Choi Young-Nae
Jung Yong-Hyun
Lee Kang-Bong
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Abstract
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An analytical method was developed for the determination of fenpropimorph, a morpholine fun- gicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhy- drous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched cali- bration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient (R2) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantifica- tion (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, LOQ×10, LOQ×50, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory val- idation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fen- propimorph residues in imported and domestic agricultural products.
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KEYWORD
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Pesticide, Fenpropimorph, Morpholine fungicide, Agricultural product, Analytical method
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