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KMID : 0881720190340010030
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Journal of Food Hygiene and Safety
2019 Volume.34 No. 1 p.30 ~ p.39
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Development and Validation of an Analytical Method for Fungicide Sedaxane Determination in Agricultural Products using LC-MS/MS
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Cho Sung-Min
Do Jung-Ah
Park Shin-Min
Lee Han-Sol
Park Ji-Su
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 sedaxane in agricultural products using liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, and then purified by using silica SPE cartridges to clean up. The analytes were quantified and confirmed by using LC-MS/MS in positive ion mode using multiple reac-tion monitoring (MRM). The matrix-matched calibration curves were linear over the calibration ranges (0.001-0.25 μg/mL) into a blank extract with r2>0.99. For validation, recovery tests were carried out at three different con-centration levels (LOQ, 10LOQ, and 50LOQ, n=5) with five replicates performed at each level. The recoveries were ranged between 74.5 to 100.8% with relative standard deviations (RSDs) of less than 12.1% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40, 2003) and Food Safety Eval-uation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for sedax-ane determination in agricultural commodities.
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KEYWORD
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Sedaxane, LC-MS/MS, Analytical method, Agricultural commodity, Fungicide
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