[1]张中华,赵亚兰.黄连总生物碱的提取纯化及含量测定[J].西部中医药,2018,31(04):49-52.
　ZHANG Zhonghua,ZHAO Yalan.Content Determination, Extraction and Purification of Total Alkaloids of HuangLian[J].Western Journal of Traditional Chinese Medicine,2018,31(04):49-52.
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黄连总生物碱的提取纯化及含量测定()
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《西部中医药》[ISSN:2096-9600/CN:62-1204/R]

卷:
31
期数:
2018年04期
页码:
49-52
栏目:
出版日期:
2018-04-15

文章信息/Info

Title:
Content Determination, Extraction and Purification of Total Alkaloids of HuangLian
文章编号:
1004-6852(2018)04-0049-04
作者:
张中华，赵亚兰
甘肃省中医院药学部，甘肃 兰州 730050
Author(s):
ZHANG Zhonghua, ZHAO Yalan
Department of Pharmacy, Gansu Provincial Hospital of Traditional Chinese Medicine, Lanzhou 730050, China
关键词:
黄连; 总生物碱; 提取纯化; 紫外-可见分光光度法
Keywords:
HuangLian;  total alkaloids;  extraction and purification;  ultraviolet-visible spectrophotometry
分类号:
R284
文献标志码:
A
摘要:
目的：:建立黄连醇提物、黄连总生物碱的提取纯化及含量测定。方法：黄连粗粉用22倍量70%乙醇提取，提取液回收乙醇，浓缩成干膏；取部分干膏用10倍量0.5%硫酸溶解、静置、过滤，酸水液加石灰乳调pH至 10～12，过滤，滤液加浓HCL调pH 为1～2，再加入药液量6%～10%的氯化钠盐析，放置，过滤，得沉淀A与滤液A；将沉淀A溶于10倍量热水，加石灰乳调pH8.5～9，趁热过滤，再将滤液加HCL调至pH 2～3，放置，过滤，沉淀水洗至中性，抽干，将得到的总生物碱反复用热水溶解处理。将滤液A加氨水调至pH 8～9，放置，过滤，再将沉淀用乙醇重结晶，得小檗胺；用紫外分光光度法定总生物碱含量。结果:得黄连干膏，黄连总生物碱(纯度为92.84%)15.8 g，小檗胺1.5 g；盐酸小檗碱在浓度为0.579 μg/mL～8.682 μg/mL 范围内，线性方程为A=81.159C-0.02 2，r=0.999 9，浓度与吸光度呈现良好的线性关系。结论:制备黄连醇提物及黄连中总生物碱的方法简便易操作;盐酸小檗碱的含量测定方法稳定性好，精密度较高，重现性好，操作简便。
Abstract:
Objective: To discuss the content determination method, extraction and purification of total alkaloids of HuangLian (rhizoma coptidis). Methods: Huanglian was extracted with 22 times 70% alcohol, alcohol was recycled in the extract , and dry paste was concentrated; part of dry paste was dissolved in ten times 0.5% sulphuric acid, left to stand and filtrated, lime milk was added till the solution shows a ph of 10~12, filtrated, concentrated HCL was added into the filtrate till the solution has a pH of 1~2, after adding 6%~10% natrium muriaticum, the solution was salted out, left to stand and filtrated, sediment A and filtrate A obtained; sediment A was dissolved in ten times hot water, to adjust PH 8.5~9 by adding lime milk, filtrated when the solution was hot, and then to adjust to pH 2~3 by adding HCL to the filtrate, the solution was left to stand, filtrated, deposited and washed to neutral, dried, the obtained total alkaloids was dissolved and handled with hot water again and again. The filtrate A was adjusted to PH8~9 after adding ammonia water, left to stand and filtrated, berbamine was obtained after the recrystallization of the sediment with ethanol; the contents of total alkaloids was detected by using ultraviolet-visible spectrophotometry. Results: HuangLian dry paste, total alkaloids of HuangLian (the purity was 92.84%) 15.8 g and berbamine (1.5 g) were obtained; the concentrations and absorbency of berberine hydrochloride showed better linear relationship when the concentrations ranged from 0.579 μg/mL to 8.682 μg/mL, linear equation was A=81.159C-0.02 2, r=0.999 9. Conclusion: The methods of preparing alcohol extract of HuangLian and total alkaloids are simple and easy to operate; the content determination method for berberine hydrochloride shows good stability, higher precision, good repeatability and easy operation.

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备注/Memo

备注/Memo:
收稿日期：2017-10-08 作者简介：张中华(1984—)，男，主管中药师。研究方向：中药质量标准研究。
更新日期/Last Update: 2018-04-15