Przyborowski L, Zawisza P, Hopkała H
Katedra i Zakład Chemii Leków Akademii Medycznej w Lublinie, ul. Okopowa 1, 20-022 Lublin.
Acta Pol Pharm. 1990;47(3-4):21-4.
Glutethimide and methyprylone were extracted from blood and plasma at pH ca. 4 (acetate buffer) thrice with chloroform, using 2.5 solvent volume ratio to that of aqueous phase. Phenobarbital was used as an internal standard in thin-layer chromatography experiments on silica gel--to obtain of comparable ratios of Rf values of glutethimide and/or methyprylone to that of phenobarbital. Suitable conditions of the separation of three substances were established using one of following mobile phases: benzene-dioxane-aq.ammonia (15:4:1), chloroform-acetone-aq.ammonia (25:25:1), chloroform-acetone-diaethylamine (5:4:1) and chloroform-diethyl ether-acetone (5:3:2); on 7.5 x 2.5 cm plates; development time (at 5 cm distance) was up to 10 minutes. The concentrations as small as 0.1 microg of examined substances in 1 cm3 of plasma may be identified on chromatograms using 20% Na2CO3 solution.
在约pH 4（醋酸盐缓冲液）的条件下，用氯仿以2.5的溶剂体积比相对于水相从血液和血浆中萃取格鲁米特和甲乙哌酮三次。在硅胶上进行薄层色谱实验时，使用苯巴比妥作为内标，以获得格鲁米特和/或甲乙哌酮与苯巴比妥的可比比移值。使用以下流动相之一建立了三种物质的合适分离条件：苯 - 二氧六环 - 氨水（15:4:1）、氯仿 - 丙酮 - 氨水（25:25:1）、氯仿 - 丙酮 - 二乙胺（5:4:1）和氯仿 - 二乙醚 - 丙酮（5:3:2）；在7.5×2.5厘米的薄板上；展开时间（在5厘米距离处）最长为10分钟。使用20%碳酸钠溶液，在色谱图上可以鉴定出血浆中每1立方厘米低至0.1微克的被测物质浓度。
