CN105232601A - Preparation method and application of decoction-free traditional Chinese fruit medicine preparation - Google Patents
Preparation method and application of decoction-free traditional Chinese fruit medicine preparation Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of traditional Chinese medicines and particularly relates to a preparation method and application of a decoction-free traditional Chinese fruit medicine preparation. The preparation method includes: subjecting traditional Chinese fruit medicines to ultrafine pulverization prior to supercritical CO2 extraction, subjecting residues left after extraction to enzymolysis, performing ultrasonic-assisted treatment and microfiltration, concentrating, drying, nano pulverizing, sterilizing and packaging to obtain the decoction-free traditional Chinese fruit medicine preparation. The preparation can be used for preparation of traditional Chinese medicine compound preparations containing the traditional Chinese fruit medicines or extracts of the traditional Chinese fruit medicines. The problems of low extraction efficiency, incompleteness in extraction of active ingredients and low utilization rate of raw materials in extraction of traditional Chinese medicines according to a conventional method are solved. The whole technical process is simple in control and environment friendly; due to synergistic interaction of steps, the preparation method is higher in extraction efficiency, active ingredients are effectively protected, and availability of the traditional Chinese fruit medicines is better improved.
Description
Technical field
The invention belongs to Chinese drug preparation technique field, be specifically related to preparation method and application thereof that a kind of fruit class Chinese crude drug exempts from decoct.
Background technology
Chinese medicine is the distinctive medicine of the Chinese tradition traditional Chinese medical science, with a long history, aboundresources.Chinese medicine ingredients complexity is various, if the process operation parameter not selecting suitable extraction, concentrated, preparation process and science strict in Chinese medicine preparation pharmacy procedure, extracts active ingredients can be caused not exclusively even to destroy effective ingredient, thus affect drug effect.The traditional dosage form of Chinese medicine has pill, powder, unguentum, medicated wine etc., but the deficiencies such as conventional dosage forms majority exists, and taking dose is large, dosage form thick, appearance poor, along with the raising of social development and people's economic level, these deficiencies have seriously constrained the paces of Chinese medicine development.Therefore, inheriting and developing on the basis of China's Advantages of TCM and characteristic, by modern high technology means, the extraction process of reform traditional, works out safety, modern Chinese medicine preparation is imperative efficiently.
Fruit class Chinese crude drug is the medical material using the fruit parts of plant as medicinal materials.Fruit class Chinese medicine is indispensable important component part in Chinese material medicine resource, and fruit apoplexy due to endogenous wind crude drug source enriches.Along with the reinforcement of health of people consciousness, application natural plant material for treating disease, health care become trend.
The preparation of Chinese medicine compound preparation generally adopts the methods such as decocting method, circumfluence method, percolation to extract, but this several extracting method temperature in leaching process raises and easily causes thermal sensitivity effective ingredient to change, and extract yield is low, extraction time is long, technique is loaded down with trivial details.Due to fruit class Chinese crude drug complex chemical composition, traditional extraction process can destroy the effective ingredient in medical material.
Summary of the invention
Technical problem to be solved by this invention is, for the deficiencies in the prior art, provides the fruit class Chinese crude drug of a kind of efficacy stability, effectively extraction and protection effective ingredient to exempt from preparation method and the application thereof of decoct.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of fruit class Chinese crude drug exempts from the preparation method of decoct, comprises the following steps:
1) fruit class Chinese crude drug is picked up clean roguing, dry;
2) dried Chinese crude drug super micron mill is ground into the Chinese crude drug fine powder that particle diameter is 100 ~ 150 μm;
3) by step 2) the Chinese crude drug fine powder that obtains puts into supercritical CO
2extract in extraction equipment, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) water of its volume 10 ~ 20 times amount is added in the medicinal residues obtained in step 3), 60 ~ 120min is soaked under 40 ~ 50 DEG C of conditions, then add the cellulase of medicinal residues weight 0.3% ~ 8% and the pectase of 0.1% ~ 0.5% carries out enzymolysis, Sonication assisted treatment, obtain extracting solution;
5) extracting solution that extract step 3) obtained and step 4) obtain merges, and carries out microfiltration process, then enters concentrator and concentrate, concentrated solution spraying dry is obtained spray drying powder;
6) spray drying powder nanometer collider pulverizing step 5) obtained, obtains nanoscale Chinese medicine microgranule, packs and obtain free decoction agent.
Preferably, supercritical CO in described step 3)
2extraction conditions is: temperature 40 ~ 50 DEG C, pressure 30 ~ 35MPa, CO
2flow velocity 12 ~ 18L/min, extraction time 2 ~ 3h.
Preferably, described step 4) cellulase enzyme activity 1 × 10
4u/g, pectase enzyme activity 1 × 10
4u/g.
Preferably, in described step 4), enzymatic hydrolysis condition is: hydrolysis temperature 40 ~ 50 DEG C, and pH is 4.0 ~ 5.8, enzymolysis time 90 ~ 180min.
Preferably, in described step 4), supersonic treatment condition is: supersonic frequency 20 ~ 25kHz, power 300 ~ 500W, time 30 ~ 40min, and number of repetition is 2 ~ 3 times.
Preferably, in described step 5), microfiltration process conditions are: filter sizes 0.2 ~ 1.2 μm, operation pressure reduction 0.08 ~ 0.15MPa.
Preferably, concentrated in described step 5) is that filtrate is carried out vacuum concentration 40 ~ 50 DEG C time, and vacuum is 0.08 ~ 0.09MPa, is concentrated into 15% ~ 25% of former filtrate volume.
Preferably, in described step 6), the particle diameter of nanoscale Chinese medicine microgranule is 40 ~ 70nm.
Present invention also offers above-mentioned preparation method gained and exempt from the application of decoct in preparation compound Chinese medicinal preparation, fruit class Chinese crude drug is exempted from decoct directly add in compound Chinese medicinal preparation, make pharmaceutically useful dosage form, described dosage form comprises decoction, granule, tablet, capsule, injection, powder, unguentum and pill.
Compared with prior art, the invention has the beneficial effects as follows:
1, the present invention adopts superfine communication technique to pulverize Chinese crude drug, sporoderm-broken rate >=95% of crude drug cell after micronizing, and powder diameter is little, is evenly distributed, and specific surface area significantly improves, and dissolving and the release of effective ingredient are accelerated.
2, the present invention adopts step by step arithmetic method to extract fruit class active ingredients from traditional Chinese medicinal.First supercritical CO is adopted
2abstraction technique extracts the oils composition contained by fruit class Chinese crude drug, supercritical CO
2the more traditional steam distillation of abstraction technique selects good separating effect, yield high, extraction temperature is lower simultaneously, extraction system seals, can protect damp and hot instability and oxidizable composition preferably, and do not adopt organic solvent, avoid organic solvent residual, there is antioxidation and sterilization functions, be conducive to ensureing and improving the quality of products; Then conbined enzymolysis is adopted to extract fruit class Chinese crude drug non-fat soluble active principals, and adopt Sonication assisted treatment, can destroy plant cell wall by enzymolysis, make the composition in plant cell more easily dissolve, spread, and combined-enzyme method is more simple, efficient, stable; The mode extracted in conjunction with ultrasonic assistant can increase molecular motion of material frequency and speed, increases solvent penetration power, improves drug-eluting speed and stripping number of times, shortens extraction time.
3, the present invention adopts micro-filter technology, and compared with conventional filtering method, microfiltration process is undergoing phase transition not, and operating condition is gentle, and be conducive to the physiologically active keeping Chinese medicine, medicinal liquid is refined, and improves concentrated and drying efficiency, improves the quality exempting from decoct.
4, the present invention adopts nano-pulverization technology, and the nano traditional Chinese medicine made exempts from the therapeutic effect that decoct can improve Chinese medicine, improves bioavailability, increases the stability of medicine, reduces dosage, reduces the toxic and side effects of Chinese medicine.
5, the present invention passes through supercritical CO
2abstraction technique, complex enzyme hydrolysis combine with technique ultrasonic assistant extract, the combination of micro-filter technology and nano-pulverization technology, solve conventional method and carry out the problems such as raw material availability low and extracts active ingredients efficiency when Chinese crude drug extracts is not high, be prepared into exempt from decoct use more convenient, more adapt to the allegro life of modern people.Whole process control of the present invention is simple, environmental protection, each processing step Synergistic; make preparation method universality of the present invention stronger; extraction efficiency is higher, and the effective ingredient of fruit class Chinese crude drug obtains and effectively extracts and protection, improves the availability of fruit class Chinese crude drug.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further elaborated.
Fruit class Chinese crude drug exempts from a preparation method for decoct, comprises the following steps:
1) fruit class Chinese crude drug is picked up clean roguing, dry;
2) dried Chinese crude drug super micron mill is ground into the Chinese crude drug fine powder that particle diameter is 100 ~ 150 μm;
3) by step 2) the Chinese crude drug fine powder that obtains puts into supercritical CO
2extract in extraction equipment, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) water of its volume 10 ~ 20 times amount is added in the medicinal residues obtained in step 3), 60 ~ 120min is soaked under 40 ~ 50 DEG C of conditions, then add the cellulase of medicinal residues weight 0.3% ~ 0.8% and the pectase of 0.1% ~ 0.5% carries out enzymolysis, Sonication assisted treatment, obtain extracting solution;
5) extracting solution that extract step 3) obtained and step 4) obtain merges, and carries out microfiltration process, then enters concentrator and concentrate, concentrated solution spraying dry is obtained spray drying powder;
6) spray drying powder nanometer collider pulverizing step 5) obtained, obtains nanoscale Chinese medicine microgranule, packs and obtain free decoction agent.
In step 1), described drying can adopt low-temperature vacuum drying, measures the water content of fruit class Chinese crude drug below 3.0% after drying with moisture test apparatus.
In step 2) in, described pulverizing can adopt Chinese medicine grinder to pulverize, and after pulverizing, Chinese crude drug is more conducive to subsequent treatment.
In step 3), described supercritical CO
2extraction conditions is: temperature 40 ~ 50 DEG C, pressure 30 ~ 35MPa, CO
2flow velocity 12 ~ 18L/min, extraction time 2 ~ 3h, supercritical CO
2the more traditional steam distillation of abstraction technique selects good separating effect, yield high; extraction temperature is lower simultaneously; extraction system seals; can protect damp and hot instability and oxidizable composition preferably; and do not adopt organic solvent; avoid organic solvent residual, there is antioxidation and sterilization functions, be conducive to ensureing and improving the quality of products.
In step 4), described cellulose enzyme vigor 1 × 10
4u/g, pectase enzyme activity 1 × 10
4u/g, described enzymatic hydrolysis condition is: hydrolysis temperature 40 ~ 50 DEG C, pH is 4.0 ~ 5.8, enzymolysis time 90 ~ 180min, enzyme has the specificity of height, destroys plant cell wall by suitable enzyme selectivity, the composition in plant cell is made more easily to dissolve, spread, mild condition, the easily removal of impurity, energy efficient, leaching rate are high, device simple, and can reduce heat-sensitive ingredients and change, and combined-enzyme method is more simple, efficient, stable.Described supersonic treatment condition is: supersonic frequency 20 ~ 25kHz, power 300 ~ 500W, time 30 ~ 40min, number of repetition is 2 ~ 3 times, the mode extracted in conjunction with ultrasonic assistant can increase molecular motion of material frequency and speed, increase solvent penetration power, improve drug-eluting speed and stripping number of times, shorten extraction time.
In step 5), described microfiltration process conditions are: filter sizes 0.2 ~ 1.2 μm, operation pressure reduction 0.08 ~ 0.15MPa, micro-filter technology is compared with conventional filtering method, microfiltration process is undergoing phase transition not, and operating condition is gentle, is conducive to the physiologically active keeping Chinese medicine, through microfiltration process, can remove the high material of the relative molecular mass mainly non-medicinal ingredient such as colloid and cellulose, extracting solution is clarified, and medicinal liquid is refined, improve concentrated and drying efficiency, improve the quality exempting from decoct.Described concentrated be that filtrate is carried out vacuum concentration 40 ~ 50 DEG C time, vacuum is 0.08 ~ 0.09MPa, is concentrated into 15% ~ 25% of former filtrate volume, and cryogenic vacuum is concentrated can reduce solvent boiling point, temperature is low, speed is fast, saves the effective ingredient of Chinese medicine extraction liquid better.
In step 6), the particle diameter of described nanoscale Chinese medicine microgranule is 40 ~ 70nm.Adopt nano-pulverization technology, the nano traditional Chinese medicine made exempts from the therapeutic effect that decoct can improve Chinese medicine, improves bioavailability, increases the stability of medicine, reduces dosage, reduces the toxic and side effects of Chinese medicine.
Present invention also offers above-mentioned preparation method gained and exempt from the application of decoct in preparation compound Chinese medicinal preparation, fruit class Chinese crude drug is exempted from decoct directly add in compound Chinese medicinal preparation, make pharmaceutically useful dosage form, described dosage form comprises decoction, granule, tablet, capsule, injection, powder, unguentum and pill.
Below by specific embodiment, those skilled in the art can be implemented.
Embodiment 1
For Fructus Corni, it exempts from the preparation method of decoct, comprises the following steps:
1) Fructus Corni is picked up clean roguing, dry;
2) dried Fructus Corni super micron mill is ground into the Fructus Corni fine powder that particle diameter is 100 ~ 150 μm;
3) by step 2) the Fructus Corni fine powder that obtains puts into supercritical CO
2extract in extraction equipment, extraction temperature 40 DEG C, pressure 30MPa, CO
2flow velocity 12L/min, extraction time 2h, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) add the water of its volume 10 times amount in the medicinal residues obtained in step 3), under 40 DEG C of conditions, soak 60min, then adding medicinal residues weight 0.3% enzyme activity is 1 × 10
4the cellulase of U/g and 0.1% enzyme activity are 1 × 10
4the pectase of U/g is 40 DEG C in temperature, and pH is enzymolysis 90min under the condition of 4.0, simultaneously Sonication assisted treatment, and supersonic frequency 20kHz, power 300W, time 30min, repeat 2 times, obtain extracting solution;
5) extracting solution that extract step 3) obtained and step 4) obtain merges, the filter membrane at room temperature carried out with aperture is 0.2 μm carries out microfiltration process, operation pressure reduction 0.08MPa, then 40 DEG C time, vacuum concentration is carried out, vacuum is 0.08MPa, be concentrated into 15% of former filtrate volume, concentrated solution spraying dry is obtained spray drying powder;
6) spray drying powder nanometer collider pulverizing step 5) obtained, obtains the nanoscale Chinese medicine microgranule that particle diameter is 40 ~ 70nm, packs and obtain free decoction agent.
Embodiment 2
For Fructus Ligustri Lucidi, it exempts from the preparation method of decoct, comprises the following steps:
1) Fructus Ligustri Lucidi is picked up clean roguing, dry;
2) dried Fructus Ligustri Lucidi super micron mill is ground into the Fructus Ligustri Lucidi fine powder that particle diameter is 100 ~ 150 μm;
3) by step 2) the Fructus Ligustri Lucidi fine powder that obtains puts into supercritical CO
2extract in extraction equipment, extraction temperature 43 DEG C, pressure 31MPa, CO
2flow velocity 13L/min, extraction time 2.5h, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) add the water of its volume 13 times amount in the medicinal residues obtained in step 3), under 43 DEG C of conditions, soak 70min, then adding medicinal residues weight 0.5% enzyme activity is 1 × 10
4the cellulase of U/g and 0.2% enzyme activity are 1 × 10
4the pectase of U/g is 43 DEG C in temperature, and pH is enzymolysis 120min under the condition of 4.5, simultaneously Sonication assisted treatment, and supersonic frequency 21kHz, power 350W, time 32min, repeat 2 times, obtain extracting solution;
5) extracting solution that extract step 3) obtained and step 4) obtain merges, the filter membrane carried out with aperture is 0.4 μm carries out microfiltration process, operation pressure reduction 0.10MPa, then filtrate is carried out vacuum concentration 43 DEG C time, vacuum is 0.085MPa, be concentrated into 17% of former filtrate volume, concentrated solution spraying dry is obtained spray drying powder;
6) spray drying powder nanometer collider pulverizing step 5) obtained, obtains the nanoscale Chinese medicine microgranule that particle diameter is 40 ~ 70nm, packs and obtain free decoction agent.
Embodiment 3
For Fructus Aristolochiae, it exempts from the preparation method of decoct, comprises the following steps:
1) Fructus Aristolochiae is picked up clean roguing, dry;
2) dried Fructus Aristolochiae super micron mill is ground into the Fructus Aristolochiae fine powder that particle diameter is 100 ~ 150 μm;
3) by step 2) the Fructus Aristolochiae fine powder that obtains puts into supercritical CO
2extract in extraction equipment, extraction temperature 45 DEG C, pressure 33MPa, CO
2flow velocity 15L/min, extraction time 2.3h, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) add the water of its volume 15 times amount in the medicinal residues obtained in step 3), under 45 DEG C of conditions, soak 80min, then adding medicinal residues weight 0.6% enzyme activity is 1 × 10
4the cellulase of U/g and 0.3% enzyme activity are 1 × 10
4the pectase of U/g is 45 DEG C in temperature, and pH is enzymolysis 140min under the condition of 5.0, simultaneously Sonication assisted treatment, and supersonic frequency 23kHz, power 400W, time 35min, repeat 3 times, obtain extracting solution;
5) extracting solution that extract step 3) obtained and step 4) obtain merges, the filter membrane carried out with aperture is 0.8 μm carries out microfiltration process, operation pressure reduction 0.12MPa, then filtrate is carried out vacuum concentration 45 DEG C time, vacuum is 0.08MPa, be concentrated into 20% of former filtrate volume, concentrated solution spraying dry is obtained spray drying powder;
6) spray drying powder nanometer collider pulverizing step 5) obtained, obtains the nanoscale Chinese medicine microgranule that particle diameter is 40 ~ 70nm, packs and obtain free decoction agent.
Embodiment 4
For Fructus Schisandrae Chinensis, it exempts from the preparation method of decoct, comprises the following steps:
1) Fructus Schisandrae Chinensis is picked up clean roguing, dry;
2) dried Fructus Schisandrae Chinensis super micron mill is ground into the Fructus Schisandrae Chinensis fine powder that particle diameter is 100 ~ 150 μm;
3) by step 2) the Fructus Schisandrae Chinensis fine powder that obtains puts into supercritical CO
2extract in extraction equipment, extraction temperature 48 DEG C, pressure 34MPa, CO
2flow velocity 16L/min, extraction time 2.8h, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) add the water of its volume 18 times amount in the medicinal residues obtained in step 3), under 48 DEG C of conditions, soak 110min, then adding medicinal residues weight 0.7% enzyme activity is 1 × 10
4the cellulase of U/g and 0.4% enzyme activity are 1 × 10
4the pectase of U/g is 48 DEG C in temperature, and pH is enzymolysis 160min under the condition of 5.3, simultaneously Sonication assisted treatment, and supersonic frequency 24kHz, power 4500W, time 38min, repeat 2 times, obtain extracting solution;
5) extracting solution that extract step 3) obtained and step 4) obtain merges, the filter membrane carried out with aperture is 1.0 μm carries out microfiltration process, operation pressure reduction 0.14MPa, then filtrate is carried out vacuum concentration 48 DEG C time, vacuum is 0.09MPa, be concentrated into 23% of former filtrate volume, concentrated solution spraying dry is obtained spray drying powder;
6) spray drying powder nanometer collider pulverizing step 5) obtained, obtains the nanoscale Chinese medicine microgranule that particle diameter is 40 ~ 70nm, packs and obtain free decoction agent.
Embodiment 5
For Fructus Amomi Rotundus, it exempts from the preparation method of decoct, comprises the following steps:
1) Fructus Amomi Rotundus is picked up clean roguing, dry;
2) dried Fructus Amomi Rotundus super micron mill is ground into the Fructus Amomi Rotundus fine powder that particle diameter is 100 ~ 150 μm;
3) by step 2) the Fructus Amomi Rotundus fine powder that obtains puts into supercritical CO
2extract in extraction equipment, extraction temperature 50 DEG C, pressure 35MPa, CO
2flow velocity 18L/min, extraction time 3h, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) add the water of its volume 20 times amount in the medicinal residues obtained in step 3), under 50 DEG C of conditions, soak 120min, then adding medicinal residues weight 0.8% enzyme activity is 1 × 10
4the cellulase of U/g and 0.5% enzyme activity are 1 × 10
4the pectase of U/g is 50 DEG C in temperature, and pH is enzymolysis 180min under the condition of 5.8, simultaneously Sonication assisted treatment, and supersonic frequency 25kHz, power 500W, time 40min, repeat 3 times, obtain extracting solution;
5) extracting solution that extract step 3) obtained and step 4) obtain merges, the filter membrane carried out with aperture is 1.2 μm carries out microfiltration process, operation pressure reduction 0.15MPa, then filtrate is carried out vacuum concentration 50 DEG C time, vacuum is 0.09MPa, be concentrated into 25% of former filtrate volume, concentrated solution spraying dry is obtained spray drying powder;
6) spray drying powder nanometer collider pulverizing step 5) obtained, obtains the nanoscale Chinese medicine microgranule that particle diameter is 40 ~ 70nm, packs and obtain free decoction agent.
Below by experiment embodiment, beneficial effect of the present invention is described.
Drug efficacy study
1, for a kind of oral traditional Chinese medicine decoction for the treatment of constipation
Chinese medicine formula: Fructus Arctii 33g, Herba Artemisiae Anomalae 12g, Radix Rehmanniae 10g, Cortex Lycii 10g, Radix Angelicae Dahuricae 12g, Poria 10g, Radix Salviae Miltiorrhizae 10g, Radix Codonopsis 10g, Herba Eupatorii 10g, Herb Gynostemmae Pentaphylli 10g, Cortex Mori 13g, Fructus Trichosanthis 10g, Semen Coicis 12g, Rhizoma Atractylodis Macrocephalae 10g, Fructus Crataegi 13g, Rhizoma Alismatis 10g, Herba Patriniae 12g.
Contrast method: get it filled with above-mentioned formula, adds in Decocting pot to decoct and makes decoction I, take according to quantity.
The inventive method 1: get Herba Artemisiae Anomalae 12g, Radix Rehmanniae 10g, Cortex Lycii 10g, Radix Angelicae Dahuricae 12g, Poria 10g, Radix Salviae Miltiorrhizae 10g, Radix Codonopsis 10g, Herba Eupatorii 10g, Herb Gynostemmae Pentaphylli 10g, Cortex Mori 13g, Rhizoma Atractylodis Macrocephalae 10g, Rhizoma Alismatis 10g, Herba Patriniae 12g add in Decocting pot to decoct and make decoction; By this method (concrete grammar is with embodiment 3), fruit class Chinese crude drug Fructus Arctii 33g, Fructus Trichosanthis 10g, Semen Coicis 12g, Fructus Crataegi 13g in formula are made and exempt from decoct; Add exempting from decoct in the decoction that all the other Chinese medicines make, stirring and dissolving, makes decoction II.
The inventive method 2: get Herba Artemisiae Anomalae 12g, Radix Rehmanniae 10g, Cortex Lycii 10g, Radix Angelicae Dahuricae 12g, Poria 10g, Radix Salviae Miltiorrhizae 10g, Radix Codonopsis 10g, Herba Eupatorii 10g, Herb Gynostemmae Pentaphylli 10g, Cortex Mori 13g, Rhizoma Atractylodis Macrocephalae 10g, Rhizoma Alismatis 10g, Herba Patriniae 12g add in Decocting pot to decoct and make decoction; Fruit class Chinese crude drug consumption in formula is reduced to Fructus Arctii 30g, Fructus Trichosanthis 9g, Semen Coicis 10g, Fructus Crataegi 11g, makes exempt from decoct by this method (concrete grammar is with embodiment 3); Add exempting from decoct in the decoction that all the other Chinese medicines make, stirring and dissolving, makes decoction III.
Lanqin oral solutions:
Choose 90 routine constipation patients, the age is all between 20 ~ 50 years old.
Above-mentioned 90 routine patients are divided into 3 groups at random, often organize 30 examples and take decoction I (matched group), decoction II (experimental group 1) and decoction III (experimental group 2) by same dose respectively, 15 days courses for the treatment of, take two courses for the treatment of continuously.
Statistics curative effect is as table 1.
Table 1 liang group Clinical efficacy comparison
As can be seen from Table 1; experimental group 1 and experimental group 2 curative effect are better than matched group; namely decoction II that this method makes is taken and decoction III curative effect is better than decoction I; decoction III curative effect when medicinal raw material consumption reduces still is better than decoction I; illustrate that fruit class Chinese crude drug prepared according to the methods of the invention exempts from the drug effect maintenance of decoct better, active component obtains effective protection and extracts.
2, for a kind of compound granule for the treatment of poliosis and increasing
Chinese medicine formula: 26 parts, Poria, Radix Polygoni Multiflori 26 parts, Radix Angelicae Sinensis 8 parts, Fructus Lycii 8 parts, Semen Cuscutae 8 parts, Radix Achyranthis Bidentatae 8 parts, Fructus Psoraleae 8 parts, Semen Sesami Nigrum 8 parts.
Contrast method: 1) lixiviate: by Chinese medicinal components remove impurity, pulverizing, puts in interlayer pot for solvent extraction, and temperature 70 C ~ 80 DEG C add 8 times of water gagings, and lixiviate 4h gets lixiviating solution and deposits; Add 8 times of water gagings again, temperature 70 C ~ 80 DEG C lixiviate 2h, merges twice decoction liquor, uses 100 mesh screen; 2) concentrate drying: filtrate is inserted in vacuum concentration pot, setting vacuum 97kPa, temperature 55 DEG C ~ 70 DEG C, be condensed into concentrated solution, concentrated solution is 25% of Chinese medicinal components, then by concentrated solution through spraying dry, obtains lixiviate powder; 3) soft material processed: lixiviate powder 40% adds in kneader, then add Mel 10%, dextrin 10%, dried starch 40%, be modulated to soft material medicine with the ethanol of content 50% and stick together; 4) granulate: adopt the extruding that sticks together of granulation machine soft material medicine to produce wet shape granule; 5) dry: wet shape granule is inserted dehydrate in 60 DEG C of pneumatic driers; 6) granulate: by dried granule after 1 10 mesh sieve granulate, obtain dissolved granule; 7) sterilization packaging: pack and obtain granule I after irradiating 2 ~ 3min under dissolved granule being inserted ultraviolet.
The inventive method 1: first fruit class Chinese crude drug Fructus Lycii 8 parts, Semen Cuscutae 8 parts, Fructus Psoraleae 8 parts, Semen Sesami Nigrum 8 parts in formula are prepared into according to the inventive method and exempt from decoct (concrete grammar is with embodiment 4); By 26 parts, Poria, Radix Polygoni Multiflori 26 parts, Radix Angelicae Sinensis 8 parts, Radix Achyranthis Bidentatae 8 parts according to contrast method step 1), step 2) process, by step 2) in gained lixiviate powder and this method gained exempt from decoct mixing, then press contrast method step 3) to step 7) process, obtain granule II.
The inventive method 2: fruit class Chinese crude drug consumption in formula is reduced to Fructus Lycii 7 parts, Semen Cuscutae 7 parts, Fructus Psoraleae 7 parts, Semen Sesami Nigrum 7 parts, is prepared into according to the inventive method and exempts from decoct (concrete grammar is with embodiment 4); By 26 parts, Poria, Radix Polygoni Multiflori 26 parts, Radix Angelicae Sinensis 8 parts, Radix Achyranthis Bidentatae 8 parts according to contrast method step 1), step 2) process, by step 2) in gained lixiviate powder and this method gained exempt from decoct mixing, then press contrast method step 3) to step 7) process, obtain granule III.
Lanqin oral solutions:
Choose 150 routine poliosis and increase patient, the age is between 15 ~ 40 years old.
Above-mentioned 150 routine patients are divided into 3 groups at random, and often organize 50 examples and take granule I (matched group), granule II (experimental group 1) and granule III (experimental group 2) by same dose respectively, continuous 20 days is a course for the treatment of, takes two courses for the treatment of continuously.
Statistics curative effect is as table 2.
Table 2 liang group Clinical efficacy comparison
As can be seen from Table 2; experimental group 1 and experimental group 2 curative effect are better than matched group; namely granule II that this method makes is taken and granule III curative effect is better than granule I; granule III curative effect when medicinal raw material consumption reduces still is better than granule I; illustrate that fruit class Chinese crude drug prepared according to the methods of the invention exempts from the drug effect maintenance of decoct better, active component obtains effective protection and extracts.
Above-mentioned clinical research can obviously be found out, fruit class Chinese crude drug prepared by the present invention is exempted from decoct and can be applied to preparation compound Chinese medicinal preparation, namely Chinese medicine decoction, granule can be prepared into, same, also can be prepared into tablet, capsule, injection, powder, unguentum and pill, not enumerate in this application; And evident in efficacy, be obviously better than conventional directly decoction gained Chinese medicine preparation.
Claims (10)
1. fruit class Chinese crude drug exempts from a preparation method for decoct, it is characterized in that, comprises the following steps:
1) fruit class Chinese crude drug is picked up clean roguing, dry;
2) dried Chinese crude drug super micron mill is ground into the Chinese crude drug fine powder that particle diameter is 100 ~ 150 μm;
3) by step 2) the Chinese crude drug fine powder that obtains puts into supercritical CO
2extract in extraction equipment, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) water of its volume 10 ~ 20 times amount is added in the medicinal residues obtained in step 3), 60 ~ 120min is soaked under 40 ~ 50 DEG C of conditions, then add the cellulase of medicinal residues weight 0.3% ~ 0.8% and the pectase of 0.1% ~ 0.5% carries out enzymolysis, Sonication assisted treatment, obtain extracting solution;
5) extracting solution that extract step 3) obtained and step 4) obtain merges, and carries out microfiltration process, then enters concentrator and concentrate, concentrated solution spraying dry is obtained spray drying powder;
6) spray drying powder nanometer collider pulverizing step 5) obtained, obtains nanoscale Chinese medicine microgranule, packs and obtain free decoction agent.
2. a kind of fruit class Chinese crude drug as claimed in claim 1 exempts from the preparation method of decoct, it is characterized in that: supercritical CO in described step 3)
2extraction conditions is: temperature 40 ~ 50 DEG C, pressure 30 ~ 35MPa, CO
2flow velocity 12 ~ 18L/min, extraction time 2 ~ 3h.
3. a kind of fruit class Chinese crude drug as claimed in claim 1 exempts from the preparation method of decoct, it is characterized in that: described step 4) cellulase enzyme activity 1 × 10
4u/g, pectase enzyme activity 1 × 10
4u/g.
4. a kind of fruit class Chinese crude drug as claimed in claim 1 exempts from the preparation method of decoct, and it is characterized in that: in described step 4), enzymatic hydrolysis condition is: hydrolysis temperature 40 ~ 50 DEG C, pH is 4.0 ~ 5.8, enzymolysis time 90 ~ 180min.
5. a kind of fruit class Chinese crude drug as claimed in claim 1 exempts from the preparation method of decoct, and it is characterized in that: in described step 4), supersonic treatment condition is: supersonic frequency 20 ~ 25kHz, power 300 ~ 500W, time 30 ~ 40min, number of repetition is 2 ~ 3 times.
6. a kind of fruit class Chinese crude drug as claimed in claim 1 exempts from the preparation method of decoct, it is characterized in that: in described step 5), microfiltration process conditions are: filter sizes 0.2 ~ 1.2 μm, operation pressure reduction 0.08 ~ 0.15MPa.
7. a kind of fruit class Chinese crude drug as claimed in claim 1 exempts from the preparation method of decoct, it is characterized in that: concentrated in described step 5) is that filtrate is carried out vacuum concentration 40 ~ 50 DEG C time, vacuum is 0.08 ~ 0.09MPa, is concentrated into 15% ~ 25% of former filtrate volume.
8. a kind of fruit class Chinese crude drug as claimed in claim 1 exempts from the preparation method of decoct, it is characterized in that: in described step 6), the particle diameter of nanoscale Chinese medicine microgranule is 40 ~ 70nm.
9. the fruit class Chinese crude drug as described in any one of claim 1 ~ 8 exempts from the application of decoct in preparation compound Chinese medicinal preparation, it is characterized in that: fruit class Chinese crude drug is exempted from decoct and directly adds in compound Chinese medicinal preparation, make pharmaceutically useful dosage form.
10. fruit class Chinese crude drug as claimed in claim 9 exempts from the application of decoct in preparation compound Chinese medicinal preparation, it is characterized in that: described dosage form comprises decoction, granule, tablet, capsule, injection, powder, unguentum and pill.
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