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KMID : 0385520140270030172
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Analytical Science & Technology
2014 Volume.27 No. 3 p.172 ~ p.180
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Development and validation of an analytical method for fungicide fenpyrazamine determination in agricultural products by HPLC-UVD
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Park Hye-jin
Do Jung-Ah
Kwon Ji-Eun
Lee Ji-Young
Cho Yoon-Jae
Kim Hee-Jeong
Rhee Gyu-Sik
Chang Moon-Ik
Oh Jae-Ho
Lee Sang-Jae
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Abstract
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Fenpyrazamine which is a pyrazole fungicide class for controlling gray mold, sclerotinia rot, and Monilinia in grapevines, stone fruit trees, and vegetables has been registered in republic of Korea in 2013 and the maximum residue limits of fenpyrazamine is set to grape, peach, and mandarin as 5.0, 2.0, and 2.0 mg/ kg, respectively. Very reliable and sensitive analytical method for determination of fenpyrazamine residues is required for ensuring the food safety in agricultural products. Fenpyrazamine residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica-SPE cartridge and eluted with hexane and acetone mixture. The purified samples were determined by HPLC-UVD and confirmed with LCMS and quantified using external standard method. Linear range of fenpyrazamine was between 0.1~5.0 μg/mL with the correlation coefficient (r) 0.999. The average recovery ranged from 71.8 to 102.7% at the spiked level of 0.05, 0.5, and 5.0 mg/kg, while the relative standard deviation was between 0.1 and 7.3%. In addition, limit
of detection and limit of quantitation were 0.01 and 0.05 mg/L, respectively. The results revealed that the developed and validated analytical method is possible for fenpyrazamine determination in agricultural product samples and will be used as an official analytical method.
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KEYWORD
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fenpyrazamine, pyrazole fungicide, HPLC-UVD, LC-MS,
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