CN100390191C - Method for extracting crude baicalin from scutellaria root - Google Patents
Method for extracting crude baicalin from scutellaria root Download PDFInfo
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- CN100390191C CN100390191C CNB2006100461179A CN200610046117A CN100390191C CN 100390191 C CN100390191 C CN 100390191C CN B2006100461179 A CNB2006100461179 A CN B2006100461179A CN 200610046117 A CN200610046117 A CN 200610046117A CN 100390191 C CN100390191 C CN 100390191C
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Abstract
The present invention relates to a method for extracting crude baicalin from scutellaria root, which relates to an extraction method of medicinal materials. The present invention particularly relates to an extraction and purification method for the effective components of traditional Chinese medicine. By using a flocculation clarification method, a scutellaria root aqueous extract liquid is processed. Before the acidic deposition, purification is carried out. Bentonite with selective adsorption action is used as a clarifying agent of the scutellaria root aqueous extract liquid. Before crude baicalin is extracted by the acidic deposition of scutellaria root aqueous extract liquid, impurities are removed by a flocculation method. For the scutellaria root aqueous extract liquid, the selective flocculation method is used for removing impurities by purification. The crude baicalin processed by bentonite as clarifying agent adopted by the present invention is brilliant yellow. The quality of the crude baicalin obtained by the present invention is obviously better than that of crude baicalin obtained by a traditional method, and the crude baicalin obtained by the present invention is suitable for medical preparation.
Description
Technical field
The present invention relates to a kind of extracting method of medicinal material, particularly relate to a kind of extraction and purifying method of middle pharmaceutically active ingredient.
Background technology
In modern Chinese herbal medicine is produced, often use the heavy method of acid from baikal skullcap root, to extract crude baicalin (main component is flavonoid compounds such as baicalin) and replace the root of large-flowered skullcap.The technology of the heavy method of acid generally is such, adds acid in root of large-flowered skullcap water extract, makes soup acidifying (the pH value generally reaches about 1.0), leaves standstill to make the precipitate precipitation, and the taking precipitate oven dry promptly obtains crude baicalin.In the heavy process of the acid of root of large-flowered skullcap water extract, some the organic macromolecule impurity in the water extract as, meetings such as pectin, starch, protein settle down with effective constituent, this just causes and contains many invalid components in the crude baicalin, has reduced drug effect.
Summary of the invention
The objective of the invention is to, process to the heavy method of root of large-flowered skullcap water extract acid is improved, before acid is heavy, use has the finings of the wilkinite of selective adsorption effect as root of large-flowered skullcap water extract, by flocculence root of large-flowered skullcap water extract is carried out defecate and purify, to remove impurity, reach the purpose of the active constituent content that improves crude baicalin.
The present invention is achieved by the following technical solutions:
Extract the method for crude baicalin in the root of large-flowered skullcap, this method comprises the steps:
The decoction of the root of large-flowered skullcap:
Baikal skullcap root decoction pieces is pulverized, and the decocting that adds 10 times of quality earlier boiled 1 hour, filtered, and the decocting that the dregs of a decoction add 8 times of quality of medicinal materials again boiled 1 hour, filtered the back merging filtrate, the corresponding approximately 0.1 gram radix scutellariae medicinal materials of every milliliter of soup this moment;
The clarification of soup:
Configuration concentration is about 10% bentonite suspension, and fully swelling is 24 hours; In the soup below 30 ℃, add volume ratio and be about 8% bentonite suspension,, treat to obtain supernatant liquor after the soup clarification by leaving standstill or centrifugal settling behind the Mixing Machine stirring 10min;
The acid of soup is heavy:
Soup after the clarification is added hydrochloric acid down at 40 ℃, soup pH value is reached about 1.0,40 ℃ of insulations were left standstill 24 hours under the normal temperature after one hour, and the throw out oven dry promptly gets comparatively purified crude baicalin.
Extract the method for crude baicalin in the aforesaid root of large-flowered skullcap, this method utilizes the flocculate and clarify method to handle root of large-flowered skullcap water extract, before acid is heavy, use wilkinite with selective adsorption effect as the finings of root of large-flowered skullcap water extract to root of large-flowered skullcap water extract purification and impurity removal.
Advantage of the present invention and effect are:
1. the finings wilkinite selected for use of the present invention has good flocculate and clarify effect to root of large-flowered skullcap water extract, and the flocculate and clarify rate reaches more than 90%.
2. wilkinite has good SELECTIVE FLOCCULATION to root of large-flowered skullcap water extract, and the root of large-flowered skullcap water extract total flavones rate of loss after the clarification is less than 4%.
3. it is heavy to carry out acid again after the use wilkinite flocculation treatment, available more purified baicalin crude product, and its active constituent content improves about 33% than former method.
4. the crude baicalin of the finings bentonite in treatment selected for use of the present invention is glassy yellow, and quality is more suitable for pharmacy significantly better than the resulting crude baicalin of traditional method.
Description of drawings
Fig. 1 is a root of large-flowered skullcap water extract colloid synoptic diagram of the present invention;
Fig. 2 is the change curve of soup foreign matter content of the present invention with pH;
Fig. 3 is that soup general flavone content of the present invention is with pH value change curve;
Fig. 4 is the flocculate synoptic diagram of colloidal solution when not adding flocculation agent in the principle of the present invention;
Fig. 5 is adsorbed on synoptic diagram on the particle for flocculate flocculation agent in the principle of the present invention;
Fig. 6 adds the synoptic diagram that flocculation agent stirs back colloidal solution for the present invention's principle of flocculating;
Fig. 7 is the preceding two kinds of different in kind pearl glue liquid solution synoptic diagram of selective flocculation of the present invention;
Fig. 8 is synoptic diagram behind the colloidal solution selective flocculation of the present invention;
Fig. 9 is the effect synoptic diagram of the power between bentonite clay particle of the present invention and the colloidal solid;
Figure 10 a is wilkinite flocculation bridge formation mode one synoptic diagram of the present invention;
Figure 10 b is wilkinite flocculation bridge formation mode two synoptic diagram of the present invention;
Figure 10 c is wilkinite flocculation bridge formation mode three synoptic diagram of the present invention;
Figure 10 d is wilkinite flocculation bridge formation mode four synoptic diagram of the present invention.
Embodiment
Method is sunk in the acid of the characteristics of root of large-flowered skullcap water extract and root of large-flowered skullcap water extract:
As scheme institute 1 and show, in root of large-flowered skullcap water extract, there is the colloidal solid of two kinds of different in kinds, effective constituent colloid and impurity colloid, wherein effective constituent colloidal granularity is much smaller than impurity colloidal granularity, among the figure: effective constituent colloidal solid 1, water 2, impurity colloidal solid 3.
Two kinds of colloidal solids its wetting ability under acidic conditions in the root of large-flowered skullcap water extract all reduces, can interosculate into larger particles by hydrophobic interaction, settle down together, shown in Fig. 2,3 (Fig. 2 herb liquid 700nm absorbance can be represented the foreign matter content of soup), the ultimate principle of the heavy method of acid that Here it is.Because the sedimentation of macromole impurity particle causes containing in the crude baicalin many impurity, before the acid of root of large-flowered skullcap water extract is heavy, remove the impurity colloid earlier and just can address this problem by the flocculate and clarify technology.
Flocculate and clarify method principle:
The flocculate and clarify technology is a kind of emerging Chinese medicine production technology, it utilizes in the nontoxic flocculation agent absorption Chinese traditional medicine water extract can not settled small impurity particle, make it to be combined into and bigger can purify Chinese traditional medicine water extract by settled floc sedimentation, shown in Fig. 4,5,6, flocculation agent is adsorbed on the colloidal solid after adding colloidal solution, forms floc sedimentation and sedimentation through mechanical dehydration (stirring).Flocculence is achieved success in some Chinese medicine productions, but also is not applied to the report that the root of large-flowered skullcap is produced.
Be insoluble in the Chinese traditional medicine water extract (effective constituent the same colloid that is with impurity in the water extract exists) of water for effective constituent, should use the purpose of the method realization removal impurity of selective flocculation, the principle of selective flocculation is shown in Fig. 7,8, a kind of colloidal solid in the flocculation agent adsorption-flocculation colloidal solution (colloidal solid) with two or more different in kinds, and keep the particle of other kind.
Wilkinite has the selective flocculation adsorption to root of large-flowered skullcap water extract:
Wilkinite has the effect of selective flocculation absorption as the finings of root of large-flowered skullcap water extract, it is flocculation absorption impurity colloidal solid only, and the effective constituent colloidal solid is not produced adsorption, thereby realized flocculating settling impurity optionally and kept the purpose of effective constituent, extracted more purified crude baicalin for the heavy method of acid condition is provided.
Wilkinite is a kind of clay class mineral of synusia shape structure, has bigger specific surface area, because special crystalline network, bentonite clay particle is electronegative.It can work to the organism in the root of large-flowered skullcap water extract by Van der Waals force and electrostatic force, and wherein Van der Waals force is relevant with the colloidal granularity, and granularity is big more, Van der Waals force is big more, and adsorptive power is strong more, and electrostatic force is relevant with the colloidal carried charge, institute's carried charge is big, and electrostatic force is just big.Impurity colloidal granularity is much larger than the effective constituent colloid in root of large-flowered skullcap water extract, two kinds of colloids are all electronegative generally speaking, the result of Van der Waals force and electrostatic force comprehensive action is exactly, the particle of wilkinite single-chip adsorbs the impurity colloid by the electrostatic force that Van der Waals force overcomes between the two, and to the effective constituent colloid because between the two electrostatic force does not produce adsorption greater than between the two Van der Waals force, so just reached the effect of impurity particle in the selective adsorption root of large-flowered skullcap water extract, as shown in Figure 9.Form floc sedimentation (wherein Figure 10 a is the basic mode that wilkinite is built bridge) by four kinds shown in Figure 10 a-10d flocculation bridge formation modes behind the wilkinite absorption impurity colloidal solid and settle down, among the figure: wilkinite single-chip 4, impurity 5.
The experimental basis of novel method:
Experiment shows that wilkinite has good flocculate and clarify effect to root of large-flowered skullcap water extract, and the flocculate and clarify rate reaches more than 90%, and simultaneously, wilkinite has good SELECTIVE FLOCCULATION to root of large-flowered skullcap water extract, and the root of large-flowered skullcap water extract total flavones rate of loss after the clarification is less than 4%.
It is heavy to carry out acid again after the use wilkinite flocculation treatment, available more purified baicalin crude product, and its active constituent content improves about 33% than former method.The total flavones yield decreases, soup total flavones yield without the wilkinite clarifying treatment is 42% with respect to root of large-flowered skullcap powder, with respect to root of large-flowered skullcap water extract is 59%, and the total flavones yield is 36% with respect to root of large-flowered skullcap powder after the bentonite in treatment, is 50% with respect to root of large-flowered skullcap water extract.
More resulting crude baicalin does not pass through the crude baicalin gray of bentonite in treatment, and is glassy yellow through the crude baicalin of bentonite in treatment, and obviously, the quality of the crude baicalin that new method makes is fit to pharmacy significantly better than traditional method.
The decoction of the root of large-flowered skullcap:
Baikal skullcap root decoction pieces is pulverized, and the decocting that adds 10 times of quality earlier boiled 1 hour, filtered, and the decocting that the dregs of a decoction add 8 times of quality of medicinal materials again boiled 1 hour, filtered the back merging filtrate, the corresponding approximately 0.1 gram radix scutellariae medicinal materials of every milliliter of soup this moment.
The clarification of soup:
Configuration concentration is about 10% bentonite suspension, and fully swelling is 24 hours.In the soup below 30 ℃, add volume ratio and be about 8% bentonite suspension,, treat to obtain supernatant liquor after the soup clarification to leave standstill or centrifugal settling behind certain speed (relevant) stirring 10min with the power of Mixing Machine.
The acid of soup is heavy:
Soup after the clarification is added hydrochloric acid down at 40 ℃, soup pH value is reached about 1.0,40 ℃ of insulations were left standstill 24 hours under the normal temperature after one hour, and the throw out oven dry promptly gets comparatively purified crude baicalin.
Claims (2)
1. extract the method for crude baicalin in the root of large-flowered skullcap, it is characterized in that this method comprises the steps:
The decoction of the root of large-flowered skullcap:
Baikal skullcap root decoction pieces is pulverized, and the decocting that adds 10 times of quality earlier boiled 1 hour, filtered, and the decocting that the dregs of a decoction add 8 times of quality of medicinal materials again boiled 1 hour, filtered the back merging filtrate, the corresponding approximately 0.1 gram radix scutellariae medicinal materials of every milliliter of soup this moment;
The clarification of soup:
Configuration concentration is about 10% bentonite suspension, and fully swelling is 24 hours; In the soup below 30 ℃, add volume ratio and be about 8% bentonite suspension,, treat to obtain supernatant liquor after the soup clarification by leaving standstill or centrifugal settling behind the Mixing Machine stirring 10min;
The acid of soup is heavy:
Soup after the clarification is added hydrochloric acid down at 40 ℃, soup pH value is reached about 1.0,40 ℃ of insulations were left standstill 24 hours under the normal temperature after one hour, and the throw out oven dry promptly gets comparatively purified crude baicalin.
2. extract the method for crude baicalin in the root of large-flowered skullcap according to claim 1, it is characterized in that, this method utilizes the flocculate and clarify method to handle root of large-flowered skullcap water extract, before acid is heavy, use wilkinite with selective adsorption effect as the finings of root of large-flowered skullcap water extract to root of large-flowered skullcap water extract purification and impurity removal.
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| CN100390191C true CN100390191C (en) | 2008-05-28 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102002082B (en) * | 2010-11-03 | 2012-09-26 | 西安赛美科医药研发有限公司 | Method for preparing baicalin |
| CN102463102B (en) * | 2010-11-16 | 2013-09-04 | 中国科学院成都生物研究所 | Surface-bonded baicalin magnetic nano-particle, and preparation method and application thereof |
| CN102617671A (en) * | 2011-01-28 | 2012-08-01 | 靳丕龙 | Method for extraction of active ingredients of baical skullcap root |
| CN103145782A (en) * | 2013-01-14 | 2013-06-12 | 李玉山 | Novel extracting process of high-purity baicalin |
| CN107349255B (en) * | 2017-07-14 | 2021-03-19 | 山东省分析测试中心 | Flocculation impurity removal process for scutellaria baicalensis extracting solution and application of flocculation impurity removal process |
| CN109320569A (en) * | 2017-08-01 | 2019-02-12 | 湘潭大学 | A method of extracting high-purity baicalin from radix scutellariae |
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Non-Patent Citations (2)
| Title |
|---|
| 黄芩苷提取液中鞣质和蛋白质的去除. 郝治湘等.齐齐哈尔大学学报，第2005卷第4期. 2005 |
| 黄芩苷提取液中鞣质和蛋白质的去除. 郝治湘等.齐齐哈尔大学学报，第2005卷第4期. 2005 * |
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