CN104887946A - Method for separating macromolecular and micromolecular active ingredients from Chinese herbal medicines once - Google Patents
Method for separating macromolecular and micromolecular active ingredients from Chinese herbal medicines once Download PDFInfo
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- CN104887946A CN104887946A CN201510341002.1A CN201510341002A CN104887946A CN 104887946 A CN104887946 A CN 104887946A CN 201510341002 A CN201510341002 A CN 201510341002A CN 104887946 A CN104887946 A CN 104887946A
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Abstract
The invention relates to a method for separating macromolecular and micromolecular active ingredients from Chinese herbal medicines once. The method comprises the following steps: the Chinese herbal medicines are smashed; deionized water is added to the smashed Chinese herbal medicines, extraction is performed for multiple times, and extracting solutions are combined; the combined extracting solution is subjected to high-speed centrifugation to obtain a supernatant liquid, the supernatant liquid is fed to a membrane separation plant, an ultrafiltration membrane is used for molecular weight cutoff, a residual liquid with larger molecular weight is dried to obtain the macromolecular active ingredients, and a dialysate with smaller molecular weight is reserved; the dialysate is loaded to a chromatographic column filled with adsorption resin for adsorption, and after saturation adsorption of the adsorption resin, 20%-80% ethanol solutions with different contents are used for gradient elution; eluents with different contents are subjected to concentration drying respectively to obtain different micromolecular active ingredients. Compared with the prior art, the method combines two Chinese herbal medicine extraction and purification methods including a membrane separation method and an adsorption resin method and achieves the purpose of obtaining of a series of high-content active ingredients through separation and purification on one assembly line.
Description
Technical field
The present invention relates to a kind of Chinese crude drug active component separation method, especially relate to a kind of disposable method isolating macromole and small molecule active composition in Chinese crude drug.
Background technology
Due to abundant functional component contained in Chinese crude drug, wherein divide by molecular weight and can be divided into Large molecule active composition and small molecule active composition two class.Because tradition is for the extraction often can only accomplished in the leaching process of Chinese crude drug a wherein class composition and the extraction that often have ignored another kind of composition, thus the effect causing Chinese medicinal material extract weakens to some extent, and the problem such as functional component content is on the low side.
Chinese patent CN 104224870 A discloses a kind of extracting method and equipment of Chinese crude drug medicinal active ingredient, extracting method is wherein that the prepared slices of Chinese crude drugs are loaded mesh bag, the mesh bag that the prepared slices of Chinese crude drugs are housed is made to form relative motion with solvent in solvent, the parts by weight ratio of solvent and medical material is 3-8: 1, Extracting temperature is between room temperature to boiling point, the movement velocity of the relative solvent of mesh bag is 20-60 m/min, extraction time 20-200 minute.Extraction equipment comprises the casing of splendid attire solvent, the cylinder in casing, and load the mesh bag of the dress prepared slices of Chinese crude drugs in cylinder, the solvent on casing adds incoming interface, solvent outlet, control device.Immersion, extraction, solid-liquid separation, medicinal residues centrifugal drying once complete continuously, eliminate medicinal residues to the pollution of environment, shorten medicine manufacturing cycle, reduce production cost, be convenient to the quality monitoring to finished product, meet the needs of new drug research and Chinese medicine production technology standardization checking.But it can not disposable separation and purification for Large molecule active composition and small molecule active composition.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and a kind of disposable method isolating macromole and small molecule active composition in Chinese crude drug is provided.
Object of the present invention can be achieved through the following technical solutions:
The disposable method isolating macromole and small molecule active composition in Chinese crude drug, comprises the following steps:
(1) Chinese crude drug is pulverized, make particle diameter reach 40-60 mesh sieve;
(2) Chinese crude drug after pulverizing adds deionized water gradation and extracts, merge extractive liquid;
(3) extracting solution is through high speed centrifugation, obtains clear liquor;
(4) first inserted in membrane separation plant by clear liquor, carry out molecular cut-off with ultrafilter membrane, the debris that molecular weight is larger carries out drying, obtains Large molecule active composition, and the peritoneal effluent of molecular weight is for subsequent use;
(5) peritoneal effluent is inserted the chromatographic column that adsorbent resin is housed to adsorb, after waiting adsorbent resin absorption saturated, carry out gradient elution by the alcoholic solution of 20-80% different content;
(6) eluent of different content is carried out concentrate drying respectively, obtain different small molecule active composition.
In step (2), total consumption of deionized water is 6 ~ 8 times of Chinese crude drug weight.
In step (3), ultracentrifugal rotating speed is 8000-10000rpm.
In step (4), ultrafilter membrane molecular cut off is 3000-5000.
Adsorbent resin described in step (5) is macroporous adsorbent resin or polyamide.
Described Large molecule active composition comprises polysaccharide and glycoprotein.
Described small molecule active composition comprises flavone or Saponin.
Described Chinese crude drug comprises Radix Ophiopogonis and Herb Gynostemmae Pentaphylli.
Compared with prior art, the present invention reaches the object that a streamline separation and purification obtains the effective ingredient of a series of high-load together with being combined with adsorption resin method two apoplexy due to endogenous wind medicinal material extract purification process by membrane separation process.The extraction ratio of the inventive method to effective ingredient is high simultaneously.Specifically, there is following beneficial effect:
(1) membrane separation process screens purification active ingredient as with molecular size range, Chinese crude drug extract in uncommon (mostly be filter clarification use, it is in the nature microporous filter membrane), and the present invention adopts membrane separation process to be separated, good separating effect.
(2) membrane separating method is combined with resin sorption processes by the present invention, can by with the disposable separation of each effective site of a collection of Chinese crude drug, and separator purity is higher, and production line efficiency is higher, reduces raw-material waste.
(3) the inventive method has stronger specific aim, can by the more effective segmentation purification of the composition of different chemical structures in large and small molecule,
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
For the extraction of the effective ingredient of Chinese crude drug Radix Ophiopogonis
To pulverize Radix Ophiopogonis and reach 40 mesh sieves, and add 8 times amount deionized waters, extract 2-3 hour, repeat 2 times, merge extractive liquid, high speed centrifugation obtains clear liquor.Clear liquor is inserted in membrane separation plant, dam with 3000 molecular weight films.Debris is dry, obtain macromolecular substances I.Peritoneal effluent is inserted adsorbent resin chromatographic column to adsorb, adsorb saturated after, the respectively eluting of the alcoholic solution with 50%, 70%, obtains small-molecule substance II, small-molecule substance III after concentrate drying.
Detect by analysis and show, macromolecular substances I is greater than the polysaccharide composition of 60% for content, and small-molecule substance II is greater than the flavonoid composition of 70% for content, and small-molecule substance III is greater than the soaping agents composition of 50% for content.
Embodiment 2
For the extraction of the effective ingredient of Chinese crude drug Herb Gynostemmae Pentaphylli
Pulverized by Herb Gynostemmae Pentaphylli and reach 60 mesh sieves, add 6 times amount, extract 3 hours, repeat 2 times, merge extractive liquid, high speed centrifugation obtains clear liquor.Clear liquor is inserted in membrane separation plant, dam with 5000 molecular weight films.Debris is dry, obtain macromolecular substances I.Peritoneal effluent is inserted adsorbent resin chromatographic column to adsorb, adsorb saturated after, the respectively eluting of the alcoholic solution with 30%, 60%, obtains small-molecule substance II, small-molecule substance III after concentrate drying.
Detect by analysis and show, macromolecular substances I is greater than polysaccharide composition and the content glycopeptide constituents complex that is greater than 20% of 50% for content; Small-molecule substance II is greater than the flavonoid composition of 50% for content; Small-molecule substance III is greater than the soaping agents composition of 80% for content.
Above-mentioned is can understand and use invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (9)
1. the disposable method isolating macromole and small molecule active composition in Chinese crude drug, is characterized in that, comprise the following steps:
(1) Chinese crude drug is pulverized;
(2) Chinese crude drug after pulverizing adds deionized water gradation and extracts, merge extractive liquid;
(3) extracting solution is through high speed centrifugation, obtains clear liquor;
(4) first inserted in membrane separation plant by clear liquor, carry out molecular cut-off with ultrafilter membrane, the debris that molecular weight is larger carries out drying, obtains Large molecule active composition, and the peritoneal effluent of molecular weight is for subsequent use;
(5) peritoneal effluent is inserted the chromatographic column that adsorbent resin is housed to adsorb, after waiting adsorbent resin absorption saturated, carry out gradient elution by the alcoholic solution of 20-80% different content;
(6) eluent of different content is carried out concentrate drying respectively, obtain different small molecule active composition.
2. the disposable method isolating macromole and small molecule active composition in Chinese crude drug according to claim 1, is characterized in that, makes particle diameter reach 40-60 mesh sieve after centering pulverizing medicinal materials.
3. the disposable method isolating macromole and small molecule active composition in Chinese crude drug according to claim 1, is characterized in that, in step (2), total consumption of deionized water is 6 ~ 8 times of Chinese crude drug weight.
4. the disposable method isolating macromole and small molecule active composition in Chinese crude drug according to claim 1, is characterized in that, in step (3), ultracentrifugal rotating speed is 8000-10000rpm.
5. the disposable method isolating macromole and small molecule active composition in Chinese crude drug according to claim 1, is characterized in that, in step (4), ultrafilter membrane molecular cut off is 3000-5000.
6. the disposable method isolating macromole and small molecule active composition in Chinese crude drug according to claim 1, is characterized in that, the adsorbent resin described in step (5) is macroporous adsorbent resin or polyamide.
7. the disposable method isolating macromole and small molecule active composition in Chinese crude drug according to claim 1, is characterized in that, described Large molecule active composition comprises polysaccharide and glycoprotein.
8. the disposable method isolating macromole and small molecule active composition in Chinese crude drug according to claim 1, is characterized in that, described small molecule active composition comprises flavone or Saponin.
9. the disposable method isolating macromole and small molecule active composition in Chinese crude drug according to claim 1, it is characterized in that, described Chinese crude drug comprises Radix Ophiopogonis and Herb Gynostemmae Pentaphylli.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510341002.1A CN104887946A (en) | 2015-06-18 | 2015-06-18 | Method for separating macromolecular and micromolecular active ingredients from Chinese herbal medicines once |
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| CN201510341002.1A CN104887946A (en) | 2015-06-18 | 2015-06-18 | Method for separating macromolecular and micromolecular active ingredients from Chinese herbal medicines once |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110624001A (en) * | 2019-10-25 | 2019-12-31 | 江西省科学院应用化学研究所 | Method for extracting polysaccharide and total flavonoids from camphor tree leaves |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202777089U (en) * | 2012-09-21 | 2013-03-13 | 南京中医药大学 | Multifunctional traditional Chinese medicine extracting, refining and concentrating equipment |
| CN103599189A (en) * | 2013-11-21 | 2014-02-26 | 贵州信邦制药股份有限公司 | Zhenqi Fuzheng (Chinese character) injection preparation and preparation method thereof |
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2015
- 2015-06-18 CN CN201510341002.1A patent/CN104887946A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202777089U (en) * | 2012-09-21 | 2013-03-13 | 南京中医药大学 | Multifunctional traditional Chinese medicine extracting, refining and concentrating equipment |
| CN103599189A (en) * | 2013-11-21 | 2014-02-26 | 贵州信邦制药股份有限公司 | Zhenqi Fuzheng (Chinese character) injection preparation and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李平华等: "大孔吸附树脂在中药有效成分分离纯化中的研究进展", 《云南中医学院学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110624001A (en) * | 2019-10-25 | 2019-12-31 | 江西省科学院应用化学研究所 | Method for extracting polysaccharide and total flavonoids from camphor tree leaves |
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Application publication date: 20150909 |
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