植物成分の微量化学的檢出法 (第7報)

ペーパークロマトグラフによる塩基類の檢出法

抄録

Paper partition chromatography was carried out using BuOH:H₂O:AcOH=5:4:1, or PhOH:H₂O:AcOH=40:9:1, as developing solvents, on over 50 kinds of basic compounds (I). Dragendorf's reagent (II), diluted to 5 volumes, was sprayed on the dried filter paper, and the spot of (I) was observed. Since some of the primary, secondary and tertiary bases do not precipitate with (II), 5% methanolic KOH and 10% methanolic solution of dimethyl sulfate are sprayed consecutively, and warmed at 70° for 5 minutes to complete N-methylation. This is sprayed with 10% acetic acid to neutralize the excess of the alkali, and (II) sprayed, by which all of (I) can be identified. The orange colored portion by (II) is a precipitate and is not washed out by water. The colored portion is cut out, extracted with a small amount of hot water, (II) added, and cooled slowly, by which orange precipitate having characteristic crystalline form can be detected under the microscope. This, therefore, is another method of identifying (I), besides its Rf value. This method is thought to have an extensive application. The authors examined methanolic extracts containing corresponding mineral acid of over 10 kinds of crude drugs containing (I) by this method and proved the presence of (I) in each.