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博落回提取物中血根碱的离子交换树脂分离纯化工艺研究
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| 篇名： | 博落回提取物中血根碱的离子交换树脂分离纯化工艺研究 |
| TITLE： | |
| 摘要： | 目的：建立博落回提取物中血根碱的离子交换树脂分离纯化工艺。方法：采用高效液相色谱法（HPLC）测定博落回提取物中血根碱含量，色谱柱为Cosmosil C18-R-Ⅱ（250 mm×4.6 mm，5 μm），流动相为乙腈-0.2％醋酸溶液（25 ∶ 75，V/V），流速为1 mL/min，检测波长为270 nm，柱温为30 ℃，进样量为20 μL。通过静态吸附与解吸附试验，对比8种离子交换树脂对血根碱的吸附和解吸附性能；采用优选离子交换树脂，考察最佳上样液浓度、上样pH值以及上样体积；采用APPS 10D液相制备系统，考察动态洗脱条件，获得博落回精提物溶液；采用反相C18色谱柱对博落回精提物溶液脱盐、洗脱并干燥，获得精制纯化物。采用HPLC法测定所得精制纯化物的纯度，并采用HPLC法、紫外分光光度法、质谱法、核磁共振法分别对其进行结构确证。结果：筛选获得CM-FF型树脂用于博落回提取物中血根碱的分离纯化，以含20％甲醇、0.25 mol/L氯化钠的20 mmol/L醋酸铵溶液100 mL进行洗脱。优化的动态吸附条件为上样浓度6.0 mg/mL、上样pH值5.5、上样体积25 mL；洗脱精提物经脱盐和精制后，最终获得纯度为97％的精制纯化产物（纯化收率为71％），并经结构确证其为血根碱。结论：优选的离子交换树脂分离纯化工艺绿色环保、安全高效、易于操作，可用于博落回提取物中血根碱单体的分离纯化，适合工业化生产。 |
| ABSTRACT： | OBJECTIVE： To establish the separation and purification technology of sanguinarine from the extract of Macleaya cordata with ion exchang resin. METHODS： The content of sanguinarine from the extract of M. cordata was determined by HPLC， with Cosmosil C18-R-Ⅱ column （250 mm×4.6 mm，5 μm）， mobile phase of acetonitrile-0.2％ acetic acid solution （25 ∶ 75，V/V）， the flow rate of 1 mL/min， detection wavelength of 270 nm， column temperature of 30 ℃， and sample size of 20 μL. Static adsorption and desorption tests were carried out to compare the adsorption and desorption properties of 8 ion exchange resins for sanguinarine. The optimum concentration of sample solution， pH value and volume of sample were investigated by optimum ion exchange resin. APPS 10D liquid phase preparation system was used to investigate the dynamic elution conditions and obtain M. cordata refined extract solution. The refined purified product of M. cordata was obtained by desalination， elution on a reversed-phase （RP） C18 column and drying. The purity of the purified product was analyzed by HPLC. The structure of the purified product was confirmed by HPLC， UV spectrophotometry， MS and NMR. RESULTS： CM-FF resin was screened for the separation and purification of sanguinarine from M. cordata extract. It was eluted with 20 mmol/L ammonium acetate solution 100 mL containing 20％ methanol and 0.25 mol/L sodium chloride. The optimal dynamic absorption condition included that the concentration of sample was 6.0 mg/mL at pH 5.0，and the loading amount was 25 mL； after desalination and refinement， for the eluted refined extract， the purified product with 97％ purity （purified yield of 71％） was obtained， and its structure was confirmed to be sanguinarine. CONCLUSIONS： The optimal separation and purification technology by ion exchange resin is green， safe， efficient and easy to operate， which can be used for the separation and purification of sanguinarine from M. cordata extract and is suitable for industrial production. |
| 期刊： | 2019年第30卷第16期 |
| 作者： | 邓霖芳，袁帅，刘江云 |
| AUTHORS： | DENG Linfang，YUAN Shuai，LIU Jiangyun |
| 关键字： | 博落回；血根碱；离子交换树脂；分离；纯化 |
| KEYWORDS： | Macleaya cordata； Sanguinarine； Ion exchange resin； Separation； Purification |
| 阅读数： | 451 次 |
| 本月下载数： | 4 次 |
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