過ヨウ素酸酸化法を利用したGuaiacol Glyceryl EtherのGas Chromatography

概要

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Pentafluorobenzyloxylamine hydrochloride (PFBOA) is an excellent reagent used for the syntheses of some derivatives in gas chromatography of water-soluble low molecular weight carbonyl compounds. To a sample solution (3.0 ml) containing 5-50μg of guaiacol glyceryl ether (GGE) 0.5 ml of 0.01 M NaIO_4 was added and the solution was oxidized on standing at room temperature for 10 minutes. After decomposing excess NaIO_4 by 0.1 N Na_2S_2O_3,HCHO produced reacted with 0.5 ml of PFBOA aqueous solution (40 mg/ml) on standing at room temperature for 60 minutes. One drop of 18 N sulfuric acid saturated with sodium chloride was further added to this solution, which was extracted with 0.3 ml of hexane containing an internal standard (IS) and applied to gas chromatography. Indobenzene (30μg/ml) and allethrin (25μg/ml) were well suited as internal standards for the determination of HCHO and methoxyphen-oxyacetaldehyde (MPA), respectively, which were both synthesized by the oxidative reaction. Gas chromatography was carried out on a glass column of 3% XE-60,2.0 m, FID and the column temperatures for HCHO and MPA were 80℃ and 190℃, respectively.
社団法人日本薬学会の論文
1982-11-25