Tjaden U R, Kraak J C, Huber J F
J Chromatogr. 1977 Mar 1;143(2):183-94. doi: 10.1016/s0378-4347(00)81823-x.
The performances of a number of liquid--solid systems, consisting of mixtures of water and methanol as liquid phase and methyl silica as solid phase, were investigated with respect to their use in the separation of barbiturates by high-pressure liquid chromatography (HPLC). Phase system selectivities and column efficiencies were determined. The results were applied to the development of a rapid method for the determination of trace amounts of barbiturates in blood. The first step in the analysis, the extraction of barbiturates from blood, was also investigated and good recoveries were achieved. The extracts were analyzed by HPLC using ultraviolet detection at 220 nm. A low detection limit and high precision were obtained; An amount of 5 ng hexobarbital, for example, can be determined with a precision of +/-15% and 5 mug with a precision of +/-0.3%. The time course of the concentration of hexobarbital in the serum and saliva of man after an oral administration of 400 mg is demonstrated.
研究了许多液固系统的性能，这些系统由水和甲醇的混合物作为液相、甲基硅石作为固相组成，考察了它们在高压液相色谱（HPLC）法分离巴比妥类药物中的应用。测定了相系统选择性和柱效。将结果应用于建立一种测定血液中痕量巴比妥类药物的快速方法。还研究了分析的第一步，即从血液中提取巴比妥类药物，并获得了良好的回收率。提取物通过HPLC在220nm处用紫外检测进行分析。获得了低检测限和高精度；例如，5ng己巴比妥可以以±15%的精密度测定，5μg可以以±0.3%的精密度测定。展示了口服400mg后人体血清和唾液中己巴比妥浓度的时间变化过程。
