本文選題：喜樹生物堿　切入點(diǎn)：毛細(xì)管電泳法　出處：《山西醫(yī)科大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：目的:本文建立了以磺丁基-β-環(huán)糊精(SBE-β-CD)和離子液體(IL)聯(lián)合作為添加劑分離分析喜樹生物堿的毛細(xì)管電泳法,并且研究了樣品在線堆積的富集方法及其在毛細(xì)管電泳分析測定喜樹生物堿中的應(yīng)用;所建立的方法簡單、方便、高效且節(jié)省有機(jī)溶劑,可用于分離測定實(shí)際樣品喜樹果和喜樹皮中的喜樹生物堿。方法:(1)以SBE-β-CD和IL聯(lián)合作為毛細(xì)管電泳背景電解質(zhì)添加劑,建立了分離喜樹生物堿的新方法,并用于實(shí)際樣品中喜樹堿的分離測定。通過考察不同濃度的緩沖溶液、p H、SBE-β-CD和IL濃度、分離電壓等對喜樹生物堿分離的影響,得到分離分析喜樹生物堿的最佳毛細(xì)管電泳條件為:未涂層熔融毛細(xì)管(50 cm×75μm,有效長度40 cm);緩沖溶液為:20 m M的硼砂溶液,20 m M SBE-β-CD,100 m M IL(p H9.0);分離電壓為15 k V,進(jìn)樣條件為:0.5 psi壓力進(jìn)樣4.0 s,檢測波長為254 nm。(2)建立了毛細(xì)管電泳大體積樣品堆積法(LVSS)分析測定微量喜樹生物堿的新方法,并以SBE-β-CD和IL聯(lián)合作為背景電解質(zhì)添加劑來分離喜樹生物堿,并將其用于實(shí)際樣品喜樹果和喜樹皮中喜樹生物堿的分離和含量測定。本文考察了緩沖溶液的濃度和p H、SBE-β-CD和離子液體(IL)濃度、分離電壓、堆積條件等的影響,優(yōu)化得到了大體積樣品堆積毛細(xì)管電泳法的最佳條件為:未涂層熔融毛細(xì)管(50cm×75μm,有效長度40 cm);最佳分離條件為25 m M的硼砂溶液(p H 9.0),20 m M SBE-β-CD,20 m M IL,分離電壓20 k V,檢測波長254 nm;最佳堆積條件為:進(jìn)樣壓力0.5 psi,進(jìn)樣時間4.0 s,反向電壓-25 k V,電極反轉(zhuǎn)時間0.17 min。結(jié)果:(1)在最佳的電泳條件下,喜樹生物堿可以在10 min內(nèi)完成分離;日內(nèi)精密度RSD4.6%,日間精密度RSD7.6%;各分析物的線性相關(guān)系數(shù)R為0.9946~0.9985;實(shí)際樣品中各分析物的平均回收率為98.8%~103.6%。(2)在最佳的毛細(xì)管電泳條件下,五種喜樹生物堿可以在20 min內(nèi)完成分離,日內(nèi)精密度RSD1.23%,日間精密度RSD3.70%;各分析物的線性相關(guān)系數(shù)R在0.9991~0.9997之間;在最佳的大體積樣品堆積條件下,分析物的富集倍數(shù)可達(dá)到5~13倍不等;實(shí)際樣品中各分析物的平均回收率為95.0%~103.2%。結(jié)論:離子液體可與環(huán)糊精聯(lián)合作為毛細(xì)管電泳背景緩沖液的添加劑,用于喜樹生物堿的分離測定;大體積樣品堆積法可用于實(shí)際樣品中含量較低的喜樹生物堿的分析測定。毛細(xì)管電泳技術(shù)為喜樹生物堿的分離與測定提供了一種更經(jīng)濟(jì)、快速、環(huán)保的新方法,離子液體與環(huán)糊精可作為分離選擇性試劑應(yīng)用于毛細(xì)管電泳分離喜樹生物堿的背景電解質(zhì)體系中。
[Abstract]:Objective: to establish a capillary electrophoresis method for the separation and analysis of camptothecin with sulfon#china_person0#-尾 -cyclodextrin (SBE- 尾 -CD) and ionic liquid (ILL) as additives. The method of sample accumulation on line and its application in the determination of camptothecin by capillary electrophoresis were studied. The method is simple, convenient, efficient and organic solvent saving. It can be used for the separation and determination of camptothecin in actual samples and bark of Camptotheca acuminata. Methods A new method for separation of camptothecin from Camptotheca acuminata was established by using SBE- 尾 -CD and IL as background electrolyte additives in capillary electrophoresis. It was applied to the separation and determination of camptothecin in practical samples. The effects of different concentrations of buffer solution, such as the concentration of SBE- 尾 -CD and IL, the separation voltage, on the separation of camptothecin were investigated. The optimum conditions for separation and analysis of camptothecin were obtained as follows: uncoated fused capillary tube 50 cm 脳 75 渭 m, effective length 40 cm ~ (-1); borax solution: 20 m M SBE- 尾 -CD1 100mm IL(p H 9.0m buffer solution; separation voltage 15 kV, sample injection. A new method for the determination of trace camptothecin was established by mass sample stacking method in capillary electrophoresis (Capillary electrophoresis), under the condition that the sample was injected under the pressure of 1: 0.5 psi for 4.0 s and the detection wavelength was 254nm.m-2). SBE- 尾 -CD and IL were used as background electrolyte additives to isolate camptotheca alkaloids. It has been applied to the separation and determination of camptothecin in actual samples and bark of Camptotheca acuminata. The effects of the concentration of buffer solution, the concentration of pHHSBE- 尾 -CD and ionic liquid (ILL), the separation voltage, the stacking conditions, etc. The optimum conditions for bulk sample stacking capillary electrophoresis were obtained as follows: uncoated fused capillary tube 50 cm 脳 75 渭 m, effective length 40 cm ~ (-1), borax solution p H 9.0 ~ 20 m ~ (-1), SBE- 尾 -CD ~ (2 +) 20 mm IL, separation voltage 20 k. V, the detection wavelength is 254 nm, the optimum packing conditions are as follows: injection pressure 0.5 psil, injection time 4.0 s, reverse voltage -25 kV, electrode reversal time 0.17 min. Camptothecin can be separated within 10 min; intra day precision RSD 4.6, day precision RSD 7.6; linear correlation coefficient R = 0.9946 ~ 0.9985; average recovery rate of analysis is 98.8 / 103.6. under the optimum conditions of capillary electrophoresis, The five camptothecins can be separated in 20 min, the intra day precision is 1.23 and the daytime precision is 3.70. The linear correlation coefficient of each analyte is between 0.9991 and 0.9997. The average recovery of each analyte was 95.0 and 103.2.Conclusion: ionic liquid and cyclodextrin can be used as additives in background buffer of capillary electrophoresis for the separation and determination of camptothecin. The bulk sample stacking method can be used for the analysis and determination of camptothecin in practical samples. Capillary electrophoresis provides a more economical, rapid and environmentally friendly method for the separation and determination of camptothecin. Ionic liquids and cyclodextrin can be used as separation selective reagents in the background electrolyte system for separation of camptotheca alkaloids by capillary electrophoresis.
【學(xué)位授予單位】：山西醫(yī)科大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O658.9;R914

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