CN101032528A - Discrete pharmaceutical technique for prescription of Chinese medicine film - Google Patents
Discrete pharmaceutical technique for prescription of Chinese medicine film Download PDFInfo
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- CN101032528A CN101032528A CN 200610057219 CN200610057219A CN101032528A CN 101032528 A CN101032528 A CN 101032528A CN 200610057219 CN200610057219 CN 200610057219 CN 200610057219 A CN200610057219 A CN 200610057219A CN 101032528 A CN101032528 A CN 101032528A
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Abstract
The present invention discloses membrane separating technology for compound Chinese medicine, and belongs to the field of pharmaceutical membrane separation technology. Water extract of compound Chinese medicine after being rough filtered is made to pass through membranes of different pore sizes or filtered molecular weights to obtain extracts of different molecular weight sections. The extracts of different molecular weight sections are then screened to determine the optimal molecular weight section with high treating effect, and the screening result is further infrared and effective liquid phase determined qualitatively and quantitatively. The present invention has the features of effective protection of the active components, simple technological process, low cost and no pollution.
Description
Technical field
The present invention relates to a kind of Chinese medicine compound membrance separation pharmaceutical technology, belong to the membrance separation pharmaceutical field.
Technical background
Change in the Chinese patent medicine preparation process at the Chinese medicine compound decoction at present, the effective site of prescription or effective ingredient when separating, are too paid attention to the problem of two aspects: what principal component is arranged in (1) prescription.(2) how these known effective sites or effective ingredient are separated.Therefore used extraction separation method all designs at this two aspect, makes Protean Chinese medicine compound follow this pattern separation and Extraction combination.The separation and extraction technology that adopts mainly contains at present: (1) carries out separation and Extraction by the difference between the chemical property of each composition, as differences such as polarity, dissolubility, Acidity of Aikalinitys.(2) membrane separation process: when having only single component, be used for separating or enrichment; And herbal mixture is usually used in remove impurity.Comprise microporous membrane filtration, ultrafiltration, hyperfiltration etc.
The problem that existing extraction separation method exists is: (1) each composition single extracts, the principle that has broken away from Chinese medicine monarch, attenuation synergistic, be difficult to reflect multicomponent, multifactorial influence in differentiation of tcm marrow and the Chinese medicine compound complex system comprehensively, make the combination that becomes simple several chemical constituents through the Chinese prescription of long-term clinical verification and meticulous compatibility, run counter to the theory of Chinese medicine.Be made up of two flavor medicines as the Chinese medicine YINHUANG KOUFUYE, find through the in-vitro antibacterial experiment: the vitro antibacterial activity of two flavor single medicinal materials is all obviously not as compound recipe.(2) the only extraction of every flavor prescription is different from the extraction of compound recipe effective ingredient, and the Chinese medicine compound composition is various, closes the interaction complexity of frying in shallow oil between each composition, or has new active component to produce, and every flavor prescription solely extracts combination and is difficult to reflect that compound recipe closes the composition variation of frying in shallow oil.As the herbal mixture SHENGMAI YIN three kinds of compositions are arranged, when wherein two kinds of composition Fructus Schisandrae Chinensis, people refer and synthesize when frying in shallow oil, because the acidity of Fructus Schisandrae Chinensis is decomposed the effective ingredient ginsenoside in the Radix Ginseng, content reduces significantly.But add another kind of composition after Radix Ophiopogonis, the ginsenoside is played significant protective effect, content improves.Illustrate that the interaction between each composition is very important in the compound recipe.(3) heating extraction repeatedly is to heat sensitive active component destructible.(4) the using and reclaiming of organic solvent, chemical reagent, consumes resources, the energy and time, contaminated environment reclaims endless, causes residual organic matter in the medicine, health risk.
Summary of the invention
A kind of Chinese medicine compound membrance separation pharmaceutical technology.The implementation step of this technology is
(1) Chinese medicine compound is closed and is fried in shallow oil, and the decocting extracting solution is removed insoluble substance by coarse filtration;
(2) with molecular weight 3000 to 5000,1000 to 3000, be divided into 3 parts below 1000, select the film in different apertures according to the size of molecular weight, with the film of medicinal liquid, descendingly filter successively by different apertures, obtain the extract of different molecular weight section;
(3) extract to the different molecular weight section carries out pharmacodynamic experiment, determines best effective molecular weight section;
(4) measure the active constituent content of best effective molecular weight section extract, measure the chemical group and the finger printing of best effective molecular weight section extract, determine quality control standard;
Described Chinese medicine compound is closed and is fried in shallow oil.
Described film can be one or more in ultrafilter membrane, NF membrane, the reverse osmosis membrane.
Described effect experiment is the Plating that adopts the in-vitro antibacterial experiment.
Effective group of the best effective molecular weight section of described mensuration extract and content are to be undertaken by analytical methods such as infrared, liquid chromatograph.
Described quality control standard is that best effective molecular weight section extract has the fingerprint collection of illustrative plates.Effectively group vibration mode and frequency of vibration on the fingerprint collection of illustrative plates as seen: stretching vibration ν
OHAt 3375-3417 centimetre
-1District, ν
CHAt 2920-2930 centimetre
-1District, ν
C=CAnd ν
C=OAt 1500-1750 centimetre
-1District, ν
C-OAt 1000-1300 centimetre
-1The district, bending vibration δ
CH3Or
CH2At 1370-1450 centimetre
-1The district.Best effective molecular weight section extract contains active ingredient chlorogenic acid and baicalin (glycosides).
Below the present invention will be further described:
Implementation step of the present invention is for extracting herbal mixture mixing decocting earlier, decocting liquid is removed insoluble substance by coarse filtration, molecular weight with the material that may exist in the medicinal liquid is divided into plurality of sections again, select ultrafilter membrane, NF membrane, the reverse osmosis membrane in different apertures according to the size of molecular weight, by the descending membrance separation that carries out successively of molecular weight, obtain the extract of different molecular weight section.Extract to the different molecular weight section, adopt Plating, carry out the pharmacodynamic experiment of in-vitro antibacterial, to determine best effective molecular weight section, then best effective molecular weight section is adopted the effective group of infrared analysis and draws finger printing, adopt high-efficient liquid phase technique to measure best effective molecular weight section extract active constituent content; Determine quality control standard.
The present invention compared with prior art has following advantage: (1) does not lose the effective active composition, comprises known, unknown or newborn active component, keeps tcm characteristic.The present invention breaks existing pattern of carrying out separation and Extraction according to known effective site or effective ingredient in the compound recipe, adopt the separation method of molecular weight segmentation combination, by be the physical characteristic of active component, guarantee that effective site known or unknown in the former Chinese medicine compound or effective ingredient do not lose, can remove impurity again.Avoided because of being subjected to existing research level and technical conditions restriction effective ingredient of the unknown and losing of newborn active component; overcome the defective that existing extractive technique becomes effective Chinese medicine compound of long-term clinical verification and meticulous compatibility simple several chemical constituents combinations; thereby protected the material base of differentiation of tcm prescription characteristic, observed theory of Chinese medical science.(2) adopt the physical property membrane separation technique, having reduced in the past, composition extracts the destruction of heating repeatedly effective ingredient.(3) improved the Chinese medicine compound quality control standard.The present invention can carry out analysis infrared, liquid chromatograph by involutory each molecular weight section of frying in shallow oil after the compound medicines liquid film separates, by qualitative and quantitative analysis to each molecular weight section, determine best film separation condition and quality control standard, thereby improved the quality control standard of Chinese medicine compound.(4) economize on resources, reduce cost, reduce pollution; The main Applied Physics method of present technique not with an organic solvent and chemical reagent, is removed from and being reclaimed and processing procedure, and reduces air and contaminated water source, and the protection environment has been avoided causing the harm of drug residue to human body not to the utmost because of chemical solvent reclaims simultaneously.(5) idea of renewal using membrane separating technology: though the membrane separation technique that the present invention adopts is a prior art, essential distinction is arranged in idea, existing technology is to determine how to carry out membrance separation according to known effective ingredient; And the present invention determines how to carry out membrance separation according to molecular weight.Molecular weight is divided into plurality of sections from big to small, and every segment molecule amount selects the film of respective aperture to separate, and reaches the purpose of the effective group of comprehensive separation compound recipe (or effective site).
Description of drawings:
Figure: the Infrared fingerprint spectra of gained YINHUANG KOUFUYE extract of the present invention
The specific embodiment:
With the YINHUANG KOUFUYE is that example elaborates to the present invention:
Embodiment 1
(1) coarse filtration: YINHUANG KOUFUYE crude drug decoction pieces is mixed, and decocting extracts, and by filter paper filtering, removes insoluble substance and gets coarse filtration liquid.
(2) segmentation fine straining: with molecular weight 3000 to 5000,1000 to 3000, be divided into the film that 3 parts are selected different apertures below 1000, by the descending ultrafilter membrane of using successively of molecular weight, membrane aperture is the 0.05-0.001 micron; NF membrane, membrane aperture are the 0.1-0.5 nanometer; Reverse osmosis membrane, 2000ppm magnesium sulfate interception capacity carries out membrance separation more than 98%.Obtain behind every group of membrane filtration concentrating and two sections fine straining liquid of dilution, three groups of films altogether 6 sections fine straining liquid.
(3) medicine efficacy screening: 6 sections fine straining liquid of gained are carried out pharmacodynamic experiment, and experimental technique is the Plating of in-vitro antibacterial experiment, and every section fine straining liquid contains the 1000mg crude drug by the 1ml extract and is mixed with and tried stock solution.Minimum inhibitory concentration contains for the 1st section and is equivalent to crude drug 4 to 8mg/ml, the 2nd section contains and is equivalent to crude drug 16 to 32mg/ml, the 3rd section contains and is equivalent to crude drug 8 to 16mg/ml, the 4th section contains and is equivalent to 8 to 16mg/ml, the 5th section contains and is equivalent to 16 to 32mg/ml, the 6th section contains and is equivalent to 1 to 2mg/ml, selects the 6th section fine straining liquid to keep as best effective molecular weight section, carries out the Quality Control analysis.
(4) Quality Control analysis: best effective molecular weight section is adopted infrared method mensuration effective group wherein, draw the fingerprint collection of illustrative plates.Effectively group vibration mode and frequency of vibration on the fingerprint collection of illustrative plates as seen: stretching vibration ν
OHAt 3375-3417 centimetre
-1District, ν
CHAt 2920-2930 centimetre
-1District, ν
C=CAnd ν
C=OAt 1500-1750 centimetre
-1District, ν
C-OAt 1000-1300 centimetre
-1The district, bending vibration δ
CH3Or
CH2At 1370-1450 centimetre
-1The district.
Finger printing is respectively 3391 ± 2 centimetres of wavelength
-1, 2932 ± 2 centimetres
-1, 1659 ± 2 centimetres
-1, 1615 ± 2 centimetres
-1, 1522 ± 2 centimetres
-1, 1450 ± 2 centimetres
-1, 1411 ± 2 centimetres
-1, 1369 ± 2 centimetres
-1, 1267 ± 2 centimetres
-1, 1186 ± 2 centimetres
-1, 1074 ± 2 centimetres
-1, 1051 ± 2 centimetres
-1, 867 ± 2 centimetres
-1, 816 ± 2 centimetres
-1, 771 ± 2 centimetres
-1, 610 ± 2 centimetres
-1There are 16 peaks at the place.
Adopt the high performance liquid chromatogram instrument to measure best effective molecular weight section active constituent content; Effective ingredient is chlorogenic acid and baicalin (glycosides).The rate of transform from compound recipe decocting liquid, chlorogenic acid is no less than 90%; Baicalin (glycosides) is no less than 84%.
Embodiment 2
(1) coarse filtration: YINHUANG KOUFUYE crude drug decoction pieces decocting is extracted,, remove insoluble substance and get coarse filtration liquid by filter paper filtering.
(2) segmentation fine straining: with molecular weight 3000 to 5000,1000 to 3000, be divided into the film that 3 parts are selected different apertures below 1000, by the descending ultrafilter membrane of using successively of molecular weight, membrane aperture is the 0.05-0.005 micron; NF membrane, membrane aperture are the 0.1-1 nanometer; Reverse osmosis membrane, 1000ppm magnesium sulfate interception capacity carries out membrance separation more than 98%.Obtain behind every group of membrane filtration concentrating and two sections fine straining liquid of dilution, three groups of films altogether 6 sections fine straining liquid.
(3) medicine efficacy screening: 6 sections fine straining liquid of gained are carried out pharmacodynamic experiment, and experimental technique is the Plating of in-vitro antibacterial experiment, and every section fine straining liquid contains the 1000mg crude drug by the 1ml extract and is mixed with and tried stock solution.Minimum inhibitory concentration contains for the 1st section and is equivalent to crude drug 4 to 8mg/ml, the 2nd section contains and is equivalent to crude drug 16 to 32mg/ml, the 3rd section contains and is equivalent to crude drug 8 to 16mg/ml, the 4th section contains and is equivalent to 8 to 16mg/ml, the 5th section contains and is equivalent to 16 to 32mg/ml, the 6th section contains and is equivalent to 1 to 2mg/ml, selects the 6th section fine straining liquid to keep as best effective molecular weight section, carries out the Quality Control analysis.
(4) Quality Control analysis: best effective molecular weight section is adopted infrared method mensuration effective group wherein, draw the fingerprint collection of illustrative plates.Effectively group vibration mode and frequency of vibration on the fingerprint collection of illustrative plates as seen: stretching vibration ν
OHAt 3375-3417 centimetre
-1District, ν
CHAt 2920-2930 centimetre
-1District, ν
C=CAnd ν
C=OAt 1500-1750 centimetre
-1District, ν
C-OAt 1000-1300 centimetre
-1The district, δ
CH3Or
CH2At 1370-1450 centimetre
-1The district.
Finger printing is respectively 3391 ± 2 centimetres of wavelength
-1, 2932 ± 2 centimetres
-1, 1659 ± 2 centimetres
-1, 1615 ± 2 centimetres
-1, 1522 ± 2 centimetres
-1, 1450 ± 2 centimetres
-1, 1411 ± 2 centimetres
-1, 1369 ± 2 centimetres
-1, 1267 ± 2 centimetres
-1, 1186 ± 2 centimetres
-1, 1074 ± 2 centimetres
-1, 1051 ± 2 centimetres
-1, 867 ± 2 centimetres
-1, 816 ± 2 centimetres
-1, 771 ± 2 centimetres
-1, 610 ± 2 centimetres
-1There are 16 peaks at the place.
Adopt the high performance liquid chromatogram instrument to measure best effective molecular weight section content of effective; Effective ingredient is chlorogenic acid and baicalin (glycosides).The rate of transform from compound recipe decocting liquid, chlorogenic acid is no less than 90%; Baicalin (glycosides) is no less than 84%.
Claims (6)
1, a kind of Chinese medicine compound membrance separation pharmaceutical technology is characterized in that:
(1) Chinese medicine compound is closed and is fried in shallow oil, and the decocting extracting solution is removed insoluble substance by coarse filtration;
(2) with molecular weight 3000 to 5000,1000 to 3000, be divided into 3 parts below 1000, select the film in different apertures according to the size of molecular weight, with the film of medicinal liquid, descendingly filter successively by different apertures, obtain the extract of different molecular weight section;
(3) extract to the different molecular weight section carries out pharmacodynamic experiment, determines best effective molecular weight section;
(4) measure the chemical group of best effective molecular weight section extract and draw finger printing, measure the active constituent content of best effective molecular weight section extract, determine quality control standard.
2, pharmaceutical technology according to claim 1 is characterized in that: described Chinese medicine compound must be closed and be fried in shallow oil.
3, pharmaceutical technology according to claim 1 is characterized in that: the film in described different apertures can be one or more in ultrafilter membrane, NF membrane, the reverse osmosis membrane.The ultrafilter membrane aperture is 0.05 to 0.001 micron; The NF membrane aperture is 0.1 to 1 nanometer; Reverse osmosis membrane, 1000 to 2000ppm magnesium sulfate interception capacities are more than 98%.
4, pharmaceutical technology according to claim 1 is characterized in that: described effect experiment is the Plating that adopts the in-vitro antibacterial experiment.Minimum inhibitory concentration is equivalent to crude drug 1 to 2mg/ml for containing.6 sections of best effective molecular weight Duan Weidi.
5, pharmaceutical technology according to claim 1 is characterized in that: the effective ingredient of the best effective molecular weight section of described mensuration extract is to be undertaken qualitative and quantitative by analytical methods such as infrared, high performance liquid chromatography.
6, pharmaceutical technology according to claim 1 is characterized in that: the quality standard of effective ingredient is:
(1) qualitative standard is the fingerprint collection of illustrative plates of infrared spectrum, and effectively group vibration mode and frequency of vibration include on the fingerprint collection of illustrative plates: stretching vibration ν
OHAt 3375-3417 centimetre
-1District, ν
CHAt 2920-2930 centimetre
-1District, ν
C=CAnd ν
C=OAt 1500-1750 centimetre
-1District, ν
C-OAt 1000-1300 centimetre
-1The district, bending vibration δ
CH3Or CH
2At 1370-1450 centimetre
-1The district.Finger printing is respectively 3391 ± 2 centimetres of wavelength
-1, 2932 ± 2 centimetres
-1, 1659 ± 2 centimetres
-1, 1615 ± 2 centimetres
-1, 1522 ± 2 centimetres
-1, 1450 ± 2 centimetres
-1, 1411 ± 2 centimetres
-1, 1369 ± 2 centimetres
-1, 1267 ± 2 centimetres
-1, 1186 ± 2 centimetres
-1, 1074 ± 2 centimetres
-1, 1051 ± 2 centimetres
-1, 867 ± 2 centimetres
-1, 816 ± 2 centimetres
-1, 771 ± 2 centimetres
-1, 610 ± 2 centimetres
-1There are 16 peaks at the place.
(2) quantitative approach adopts high-efficient liquid phase technique, and quality standard is that effective ingredient is chlorogenic acid and baicalin (glycosides).The rate of transform of effective ingredient from compound recipe decocting liquid in the optimum weight section, chlorogenic acid is no less than 90%; Baicalin (glycosides) is no less than 84%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610057219 CN101032528A (en) | 2006-03-09 | 2006-03-09 | Discrete pharmaceutical technique for prescription of Chinese medicine film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200610057219 CN101032528A (en) | 2006-03-09 | 2006-03-09 | Discrete pharmaceutical technique for prescription of Chinese medicine film |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837047A (en) * | 2010-06-01 | 2010-09-22 | 河南百年康鑫药业有限公司 | Method for preparing concentrated Yinhuang oral liquid |
| CN109012185A (en) * | 2018-08-23 | 2018-12-18 | 河北维尔利动物药业集团有限公司 | Membrane separation technique takes orally the application in liquid preparing process in cordate houttuynia a kind of reed mentioned in ancient books indigo plant |
| CN111991525A (en) * | 2020-09-02 | 2020-11-27 | 中国药科大学 | Effective component group of Simiao pills and preparation method and application thereof |
| CN113477084A (en) * | 2021-08-12 | 2021-10-08 | 广州高得环保科技股份有限公司 | Automatic control method and system for pipeline direct drinking water film filtration |
-
2006
- 2006-03-09 CN CN 200610057219 patent/CN101032528A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837047A (en) * | 2010-06-01 | 2010-09-22 | 河南百年康鑫药业有限公司 | Method for preparing concentrated Yinhuang oral liquid |
| CN109012185A (en) * | 2018-08-23 | 2018-12-18 | 河北维尔利动物药业集团有限公司 | Membrane separation technique takes orally the application in liquid preparing process in cordate houttuynia a kind of reed mentioned in ancient books indigo plant |
| CN111991525A (en) * | 2020-09-02 | 2020-11-27 | 中国药科大学 | Effective component group of Simiao pills and preparation method and application thereof |
| CN111991525B (en) * | 2020-09-02 | 2022-05-03 | 中国药科大学 | Effective component group of Simiao pills and preparation method and application thereof |
| CN113477084A (en) * | 2021-08-12 | 2021-10-08 | 广州高得环保科技股份有限公司 | Automatic control method and system for pipeline direct drinking water film filtration |
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