Development and Validation of an Analytical Method for Determination of Fungicide Tridemorph in Agricultural Commodities Using LC-MS/MS
2017
Pak, W.M., Ministry of Food and Drug Safety, Cheongju, Republic of Korea | Do, J.A., Ministry of Food and Drug Safety, Cheongju, Republic of Korea | Lim, S.H., Ministry of Food and Drug Safety, Cheongju, Republic of Korea | Park, S.M., Ministry of Food and Drug Safety, Cheongju, Republic of Korea | Yoon, J.H., Ministry of Food and Drug Safety, Cheongju, Republic of Korea | Lee, D.S., Korea Advanced Food Research Institute, Uiwang, Republic of Korea | Chang, M.I., Audit and Inspection Office, Ministry of Food and Drug Safety, Cheongju, Republic of Korea
The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl (NH2) SPE catridge. The purified samples were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~2.5 ng) into a blank extract with r²greater than 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, 10 x LOQ, 50 x LOQ, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.
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