次亜鉛素第三ブチルを用いるアミド基、イミド基、あるいはアミノ基を有する医薬品の薄層クロマトグラム上における微量検出法

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The plate was prepared with Silicagel G, Merck Co., suspended in 1.5% aqueous soluble starch solution. It was activated at 90℃ for 1 h. Following solvent systems were employed in the development: A, petrokeyn ether-acetone-methylethylketone (8:1:1); B, chloroform-acetone (9=1); C, cyclohexane-acetone (3:1); D, carbon tetrachloride-99% ethanol (8:1); E, 99% ethanol-acetic acid-water (5:0.1=2); F, 99% ethanol-water (5:2). Solvent system A and B were proved to be excellent for the separation of amides and imides tested. Solvent system E was suitable for antibiotics. The plate was dried at 100℃ for 15min when the solnvents A-D were used for 30 min when solvents E and F were used. The dried plate was placed in a Petri dish in which two drops of 10% tert-butyl hypochlorite in acetic acid had previouoly been added. The plate was supported by a twisted glass rod and its silicagel layer should be faced towards the bottom of the dish to assure fast reaction with the vapor of the reagent. The Petri dish was immediately covered with its lid and allowed to stand for 2min. The plate was then taken out and left for 1Omin at room temperature to remove excess hypohlrite. The plate was sprayed with 1% potassium iodide to give blue-brown spots on a almost colorless background. The color was stable overnight when the layer was covered with polyethylene film. The present method was found to be markedly sensitive and simple. Limits of detection for barbiturates and hydantoins tested were 10ng. On the other hand, antibiotics having amino sugar moieties showed limit of detection of 400ng.
社団法人日本分析化学会の論文
1975-02-10

次亜鉛素第三ブチルを用いるアミド基、イミド基、あるいはアミノ基を有する医薬品の薄層クロマトグラム上における微量検出法

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