生体試料中のシクロヘキシルアミンの螢光定量法

概要

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A method for fluorometric determination of cyclohexylamine, a metabolite of cyclamate, in biological samples was devised. Cyclohexylamine was extracted with 5 ml of chloroform from 3-5 ml of the sample (urine, blood, or tissue homogenates) basified to pH 13 with 6 N NaOH. Then, 4 ml of the chloroform layer was shaken with 4 ml of 0.5 N HCl. To 1 ml of the aqueous layer, 0.08 ml of 6 N NaOH, 0.92 ml of water, 2 ml of 0.5% 1-dimethyl-aminonaphthalene-5-sulfonyl chloride in acetone, and 1 ml of 5% NaHCO_3 were added. The sample was kept at a room tempeature overnight, and shaken with 5 ml of chloroform. After 6 ml of the chloroform-acetone layer was concentrated in vacuo, the volume was adjusted to 1.5 ml with acetone. Then, 0.1 ml of the concentrate was spotted on silica gel plate and developed with a mixture of benzene : acetone (20 : 1). A yellow fluorescent spot (Rf 0.6) was extracted with 4 ml of dioxane and fluorescence (ex. 360 mμ, fl. 490 mμ, excited with Hg lamp) was estimated. The standard curve was linear within the range of 0.5-5 μg/ml and the recovery from urine, blood, or tissue homogenates of guinea pig and human urine was satisfactory.
公益社団法人日本薬学会の論文
1972-04-25