高效毛细管电泳技术在结构相似药物分离分析中的应用研究

发布时间：2018-06-20 00:00

  本文选题：高效毛细管电泳 + 环糊精　； 参考：《山西医科大学》2017年硕士论文

【摘要】：目的:本文第一部分采用环糊精衍生物为毛细管电泳的背景电解质添加剂,旨在建立一种简单、快速的分离螺内酯与坎利酮的毛细管电泳新方法,并将其应用于螺内酯制剂及尿液基质中螺内酯和坎利酮的分析。本文第二部分采用二元环糊精体系,研究其对四种钩藤生物碱拆分的影响,旨在建立一种高效、环保的毛细管电泳新方法,并将其应用于钩藤药材及制剂中钩藤生物碱的分离测定。方法:采用贝克曼毛细管电泳仪,二极管阵列检测器,通过考察吸收波长,背景电解质溶液浓度、添加剂种类及浓度、pH以及分离电压对待测化合物分离的影响,最终得出:(1)同时分离测定螺内酯与坎利酮的最优电泳条件为:未涂层毛细管柱(75μm×57cm,有效长度50 cm);以含4.5 g/L磺酸基-β-环糊精的磷酸盐缓冲液(20 m M,pH5.5)为背景电解质溶液;分析电压15 k V;检测波长260 nm;进样条件:0.5 psi,5 s;以醋酸氟轻松为内标,使用内标法对螺内酯及坎利酮进行含量测定。(2)同时分离测定四种钩藤生物碱的最优电泳条件为:未涂层毛细管柱(75μm×30.3 cm,有效长度20.2 cm);以含161.7 m M羟丙基-β-环糊精和2.21 m M乙二胺基-β-环糊精的磷酸盐缓冲液(40 m M,pH 5.7)为背景电解质溶液;分析电压15 k V;温度25℃,检测波长250 nm,进样条件:0.5 psi,5 s。结果:在最佳毛细管电泳条件下,螺内酯与坎利酮的线性关系良好,相关系数R为0.9976-0.9997;分析物可在7 min内完成分离,分离度为3.6;日内精密度2.9%,日间精密度4.3%;实际样品的回收率在99.0-106.8%之间。在最佳毛细管电泳条件下,四种钩藤生物碱的线性关系良好,相关系数R为0.9992-0.9995;分析物可在13 min内完成分离,分离度在2.2-8.3之间;四种钩藤生物碱的日内精密度3.8%,日间精密度5.0%;实际样品的回收率在96.2-106.0%之间。结论:使用毛细管电泳技术可对结构相似的化合物螺内酯和坎利酮进行分离测定。所建立的毛细管电泳新方法操作简便,可用于螺内酯制剂的含量测定及尿液中螺内酯和坎利酮的分析。将二元环糊精体系应用于毛细管电泳对四种结构相似的钩藤类生物碱进行分离测定。所建立的毛细管电泳新方法操作简单方便,可用于钩藤药材及制剂中主要钩藤生物碱的含量测定。
[Abstract]:Objective: in the first part of this paper, cyclodextrin derivatives were used as background electrolyte additives in capillary electrophoresis to establish a simple and rapid capillary electrophoresis method for the separation of spironolactone and Canlidone. It was applied to the analysis of spironolactone and canalidone in spironolactone preparation and urine matrix. In the second part of this paper, the effects of binary cyclodextrin system on the separation of four alkaloids were studied. The aim of this study was to establish a new method of capillary electrophoresis with high efficiency and environmental protection. It was applied to the separation and determination of the alkaloids in the medicinal materials and preparations of Uncaria tenuifolia. Methods: Beckmann capillary electrophoresis apparatus and diode array detector were used to investigate the effects of absorption wavelength, concentration of background electrolyte solution, kinds and concentrations of additives, pH and separation voltage on the separation of compounds. The optimal conditions for simultaneous separation and determination of spironolactone and canalidone were obtained as follows: uncoated capillary column 75 渭 m 脳 57 cm, effective length 50 cm ~ (-1), phosphate buffer containing 4.5 g / L sulfonic acid-尾 -cyclodextrin, pH 5.5). Analytical voltage 15 kV; detection wavelength 260 nm; sample injection condition: 0.5 psir 5 s; fluoride acetate as internal standard, The optimum electrophoretic conditions for simultaneous separation and determination of four alkaloids were as follows: uncoated capillary column 75 渭 m 脳 30. 3 cm, effective length 20. 2 cm ~ (-1), hydroxy propyl-尾-cyclodextrin with 161.7 mm. 2.21 mm ethylenediamide- 尾 -cyclodextrin phosphate buffer (40 m Mm) was used as the background electrolyte solution. The analytical voltage is 15 kV, the temperature is 25 鈩，

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