反相高效液相色谱同时测定复方降压药中三组分

建立了一种反相高效液相色谱法 ,用于同时测定复方降压药中三组分。采用YWGC1 8柱 ,以甲醇 醋酸 醋酸钠缓冲液 水 ( 60∶2 0∶2 0 )为流动相 ,流速为 0 .8mL·min- 1 ,二极管阵列检测器于检测波长 2 60nm测定。硫酸双肼酞嗪、氢氯噻嗪和氨苯喋啶的线性范围分别为 0 .0 8～ 1 .1mg/mL ,0 .0 1～ 0 .30mg/mL ,0 0 3～ 0 .45mg/mL ,检测限分别为 0 0 0 6mg/mL ,0 0 0 1mg/mL ,0 0 0 1mg/mL ,已用于北京降压0号样品的测定     

Subunit structure of glycinin and its molecular species based on RP-HPLC, gel electrophoresis and SEC studies

Glycinin and its molecular species (glycinin I and glycinin II) were separated and isolated. The number and kind of subunits of glycinin, glycinin I and glycinin II were determined. Studies were carried out under different experimental conditions using slab gel electrophoresis, size-exclusion chromatography and reversed-phase high performance liquid chromatography. Gel electrophoresis was done using both continuous and discontinuous system and under varying concentrations of resolving gel. In addition, the subunits were separated by reversed phase using gradient program. Glycinin and glycinin II were found to have 12 subunits each while glycinin I showed six subunits. Molecular weight and weight ratio in each case were also determined.     

山东不同产地丹参的HPLC指纹图谱-化学模式识别研究

建立RPHPLC指纹图谱-化学模式识别评价丹参质量的方法.利用RPHPLC法测定不同产地丹参药材的指纹图谱及丹参酮ⅡAt和丹参酮的含量,采用主成分分析、系统聚类分析和逐步判别分析对指纹图谱信息进行化学模式识别研究.在主成分分析的基础上,以前4个主成分为聚类分析的指标进行系统聚类分析,取阈值为8时,所有样品可被分为4类;并建立了相应的判别函数,回判准确率100%;以此为依据,初步建立了丹参化学模式识别的评价方法.     

Optimization of a multisolvent composition in RPHPLC: Generalization to non- ideal peaks

Summary When samples contain solutes at very different concentrations, the use of the classical resolution function to express the quality of the separation does not provide a true measure of peak overlap and is therefore unsuitable for optimization. Apart from this case, the validity of the optimum is highly dependent on the accuracy of the predicted retention surfaces and it is essential to restrict the parameter space in which optimum performance is sought. As a result, most interpretive optimization procedures become unreliable for optimizing the composition of multisolvent systems in RPHPLC, particularly for non-ideal peaks. These difficulties can be overcome by the method proposed here: the ability, by means of a criterion, called CRIT, to select a restricted range of composition in order to enhance the accuracy of the response surface is developed for non-ideal peaks. The best composition within this selected range is then determined by using a modified resolution function. The performance of this procedure is discussed with some illustrative examples.