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KMID : 0881720180330040296
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Journal of Food Hygiene and Safety
2018 Volume.33 No. 4 p.296 ~ p.305
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Development and Validation of Analytical Method for Determination of Fungicide Spiroxamine Residue in Agricultural Commodities Using LC-MS/MS
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Park Shin-Min
Do Jung-Ah
Lim Seung-Hee
Yoon Ji-Hye
Pak Won-Min
Shin Hye-Sun
Kuk Ju-Hee
Chung Hyung-Wook
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Abstract
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Spiroxamine, one of fungicides, is used to control powdery mildew in various crops and black yellow sigatoka in bananas. The major strength of spiroxamine is to control powdery mildew in various crops and bananas yellow sigatoka in bananas. The compound has shown a high level of activity, good persistence and crop tolerance. Besides powdery mildew, good control of rust, net blotch and Rhynchosporium diseases been indicated in cereals, together with a complementary activity against Septoria diseases. In 2017, the maximum residue limit (MRL) of spiroxamine established in Korea. According to Ministry of ood and rug afety) regulations, spiroxamine residues defined only parent compound. Thus, a analytical method is needed to estimate the residue level of the parent compound. The objective of this study was to develop and validate analytical method for spiroxamine in representative agricultural commodities. Samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interfering substances. The analyte were quantified and confirmed 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 (0.0005~0.1 μg/mL) for the analyte in blank extract with coefficient of determination (r2) > 0.99. For validation purposes, recovery studies will be carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries 70.6~104.6% with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges in the Codex guidelines (CAC/GL40, 2003) and MFDS guidelines. proposed analytical method be used as an official analytical method in the Republic of Korea.
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KEYWORD
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Spiroxamine , Fungicide , LC-MS/MS , Analytical method , Agricultural commodities
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