超臨界流体抽出/超臨界流体クロマトラグフィー直接導入法によるビタミンKの分析(<特集>医薬品の分析)

概要

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We have already reported the new double-stage separation method which combines supercritical fluid extraction (SFE) directly with supercritical fluid chro- matography (SFC). The new SFE/SFC method incorporates SFE as the first separation step and SFC as the second separation step. This arrangement allows the analyst to apply raw and solid samples directly to the system. In addition, the use of SFE/SFC enables true SFC which is not affected by the solvent, that often plays a role of modifier only for early eluting peaks, used for dissolving samples. Here, application of this method to the analysis of vitamin Ks is described. A solution of vitamins K_1, K_2 and K_3 were dried on a piece of filter paper, then applied to the SFE/SFC system. Stopped-flow extraction was performed at 40℃ with 200 bar pressure for 2.5 min, then the extract was directly introduced into the SFC system. All the three vitamins were completely separated on a silica gel column within 4.5 min using supercritical carbon dioxide (2.0 l/min) with acetonitrile (0.1 ml/min) as a modifier. The relative standard deviation of the retention times was less than 2.0% for ten consecutive runs.
社団法人日本分析化学会の論文
1986-03-05