高速液体クロマトグラフィーによる飼料中のモネンシンの定量

概要

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A facile and rapid method for the determination of monensin in feeds by HPLC was reported. Solid phase extraction of monensin in a feed, followed by derivatization with 9-anthryldiazomethane (ADAM) was carried out. The monensin-ADAM derivative was determined with a fluorescence detector. Monensin in a feed was extracted from a mixture of methanol and acetone (9 : 1) and then the extract was filtered under reduced pressure. After the extract was evaporated to dryness, the residue was dissolved by methanol and then the solution was centrifuged for 5 min. The resulting supernatant was applied to a ODS cartridge column (Bond Elut C_<18>), followed by washing with 20% aqueous methanol sloution and then eluting with 90% aqueous methanol to obtain the monensin fraction. Monensin in the eluent was converted into the corresponding ADAM-monensin derivative by reaction with the ADAM reagent in the presence of crown ether for 2 h at room temperature. The reaction mixture was injected to the analytical column. The conditions of HPLC was as followed ; column, Shim-pack CLC-ODS (6.0 mm i. d. ×150 mm L) ; mobile phase, 10 mM magnesium acetate in 95% aqueous methanol : flow rate, 1.4 ml/min : column temp., 45℃ detector, RF-535 (Ex 365 nm, Em 412 nm). The calibration curve was linear from 0.1 μg/ml to 1.5 μg/ml. Recoveries of monensin added to the feed at the level of 10 μg/ml were 82.8+2.1% (n=5).
社団法人日本分析化学会の論文
1988-06-05