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KMID : 0385520140270050234
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Analytical Science & Technology
2014 Volume.27 No. 5 p.234 ~ p.242
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Development and validation of an analytical method for nematicide imicyafos determination in agricultural products by HPLC-UVD
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Do Jung-Ah
Park Hye-jin
Kwon Ji-Eun
Oh Jae-Ho
Hogn Jin-Hwan
Chang Moon-Ik
Choe Won-Jo
Lee Hyun-Sook
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Abstract
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Imicyafos which is a nematicide for controlling root-knot nematodes has been registered in the Republic of Korea in 2012, and the maximum residue limits of imicyafos are set to watermelon and korean melon as each 0.05 mg/kg. Extremely reliable and sensitive analytical method is required for ensuring food safety on imicyafos residues in agricultural commodities. Imicyafos residues in samples were extracted with acetone, partitioned with hexane and dichloromethane, and then purified with florisil. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. Linear range was between 0.1~5 mg/kg with the correlation coefficient (r2) 0.99997. Average recoveries of imicyafos ranged from 77.0 to 115.4% at the spiked levels of 0.02 and 0.05 mg/kg with the relative standard deviations of 2.2~9.6%. Limit of detection and
quantification were 0.005 and 0.02 mg/kg, respectively. An inter-laboratory study was conducted to validate the determination method in depth, and the results were satisfactory. All of the validation results revealed that the developed analytical method in this study is relevant for imicyafos determination in agricultural commodities and will be used as an official analytical method.
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KEYWORD
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imicyafos, nematicide, HPLC-UVD, LC-MS, official analytical method,
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