本文選題：高效毛細(xì)管電泳 + 環(huán)糊精��； 參考：《山西醫(yī)科大學(xué)》2017年碩士論文

【摘要】：目的:本文第一部分采用環(huán)糊精衍生物為毛細(xì)管電泳的背景電解質(zhì)添加劑,旨在建立一種簡單、快速的分離螺內(nèi)酯與坎利酮的毛細(xì)管電泳新方法,并將其應(yīng)用于螺內(nèi)酯制劑及尿液基質(zhì)中螺內(nèi)酯和坎利酮的分析。本文第二部分采用二元環(huán)糊精體系,研究其對四種鉤藤生物堿拆分的影響,旨在建立一種高效、環(huán)保的毛細(xì)管電泳新方法,并將其應(yīng)用于鉤藤藥材及制劑中鉤藤生物堿的分離測定。方法:采用貝克曼毛細(xì)管電泳儀,二極管陣列檢測器,通過考察吸收波長,背景電解質(zhì)溶液濃度、添加劑種類及濃度、pH以及分離電壓對待測化合物分離的影響,最終得出:(1)同時分離測定螺內(nèi)酯與坎利酮的最優(yōu)電泳條件為:未涂層毛細(xì)管柱(75μm×57cm,有效長度50 cm);以含4.5 g/L磺酸基-β-環(huán)糊精的磷酸鹽緩沖液(20 m M,pH5.5)為背景電解質(zhì)溶液;分析電壓15 k V;檢測波長260 nm;進(jìn)樣條件:0.5 psi,5 s;以醋酸氟輕松為內(nèi)標(biāo),使用內(nèi)標(biāo)法對螺內(nèi)酯及坎利酮進(jìn)行含量測定。(2)同時分離測定四種鉤藤生物堿的最優(yōu)電泳條件為:未涂層毛細(xì)管柱(75μm×30.3 cm,有效長度20.2 cm);以含161.7 m M羥丙基-β-環(huán)糊精和2.21 m M乙二胺基-β-環(huán)糊精的磷酸鹽緩沖液(40 m M,pH 5.7)為背景電解質(zhì)溶液;分析電壓15 k V;溫度25℃,檢測波長250 nm,進(jìn)樣條件:0.5 psi,5 s。結(jié)果:在最佳毛細(xì)管電泳條件下,螺內(nèi)酯與坎利酮的線性關(guān)系良好,相關(guān)系數(shù)R為0.9976-0.9997;分析物可在7 min內(nèi)完成分離,分離度為3.6;日內(nèi)精密度2.9%,日間精密度4.3%;實(shí)際樣品的回收率在99.0-106.8%之間。在最佳毛細(xì)管電泳條件下,四種鉤藤生物堿的線性關(guān)系良好,相關(guān)系數(shù)R為0.9992-0.9995;分析物可在13 min內(nèi)完成分離,分離度在2.2-8.3之間;四種鉤藤生物堿的日內(nèi)精密度3.8%,日間精密度5.0%;實(shí)際樣品的回收率在96.2-106.0%之間。結(jié)論:使用毛細(xì)管電泳技術(shù)可對結(jié)構(gòu)相似的化合物螺內(nèi)酯和坎利酮進(jìn)行分離測定。所建立的毛細(xì)管電泳新方法操作簡便,可用于螺內(nèi)酯制劑的含量測定及尿液中螺內(nèi)酯和坎利酮的分析。將二元環(huán)糊精體系應(yīng)用于毛細(xì)管電泳對四種結(jié)構(gòu)相似的鉤藤類生物堿進(jìn)行分離測定。所建立的毛細(xì)管電泳新方法操作簡單方便,可用于鉤藤藥材及制劑中主要鉤藤生物堿的含量測定。
[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，

本文編號：2041938