Thin-layer chromatography on silica gel and alumina sintered sticks

OKUMURA Tamotsu, KADONO Tetsuro

doi:10.2116/bunsekikagaku.22.980

In a previous paper we reported the preparation of the silica gel and alumina sintered plates. They consited of a layer of silica gel or alumina on various kinds of glass or metal base plate fixed with several kinds of sintered glass powder.<BR>In the present paper we reported that the previously reported welding procedure was successfully applied to the preparation of silica gel or alumina sintered sticks. As reported previously, several kinds of glass or metal sticks were used as support and several kinds of glass powder were tested as binders. While these three materials are very much different from each other in their expansion coefficient (α) as shown in Table I, the welding among these materials does occur.<BR>Thin-layer chromatographic separation of the following test mixtures was performed by using these silica gel and alumina sintered sticks: azodyes (indophenol, Sudan red G and p-dimethylaminoazobenzene, and p-aminoazobenzene, Sudan yellow and azobenzene), estrogens (estriol, estradiol and estrone), alkaloids (quinine, codeine, brucine and thebaine)and lipids (cholesterol, cholesteryl stearate, monostearin, distearin, tristearin, stearic acid and methyl oleate). All these sticks are thermo-stable, and those with glass stick supports are acid-resistant and, moreover, can be repeatedly used without reactivation after being in the hydrogen flame ionization detector. As shown in Table IV and IX, these sintered sticks have very superior reproducibility of separation.<BR>By using the silica gel quartz sintered sticks, a quantitative determination of lipids was attempted. Among the five kinds tested, two kinds of stick with glass ceramic or borosilicate as binder were proved to be useful owing to their small baseline noise in response (Fig. 3 and 4). The response reproducibility of lipids was very good when scanning was performed with TLC-flame ionization detector (FID). The coefficient of variation was less than 5% in three weight ratios (Table VIII).<BR>The silica gel sintered sticks and thd silica gel Laboratorymade sticks when used together with TLC-FID apparatus will facilitate the qualitative and quantitative analysis of lipids in biological fluids, heavy oil fractions in petroleum industry and plant components in phytochemistry.

Thin-layer chromatography on silica gel and alumina sintered sticks

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