CN105125637A - Preparing method for flower traditional Chinese medicinal material decoction-free preparation and application thereof - Google Patents
Preparing method for flower traditional Chinese medicinal material decoction-free preparation and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of traditional Chinese medicine preparing, and particularly relates to a preparing method for a flower traditional Chinese medicinal material decoction-free preparation and an application thereof. The preparing method includes the steps that after flower traditional Chinese medicinal materials are smashed, supercritical CO2 extraction is carried out; ultrasonic-assisted alcohol extraction is carried out, and ultrasonic-microwave cooperation extraction is carried out; then microfiltration treatment is adopted, finally concentrating, drying, nanometer smashing and packaging are carried out, and the flower traditional Chinese medicinal material decoction-free preparation is obtained. The preparation can be used for preparing a Chinese herbal medicine compound preparation containing flower traditional Chinese medicinal materials or flower traditional Chinese medicinal material extract. By means of the preparing method, the problems that when traditional Chinese medicinal material extraction is carried out with a conventional method, the raw material use rate is low, extraction of effective ingredients is incomplete, and extracting efficiency is low are solved; the whole technological process is easy to control and environmentally friendly, and technological steps synergistic interact with each other, so that the extracting efficiency of the preparing method is higher, the effective ingredients are effectively protected, and the utilization degree of the flower traditional Chinese medicinal materials is increased.
Description
Technical field
The invention belongs to Chinese drug preparation technique field, be specifically related to a kind of spend class Chinese crude drug to exempt from decoct preparation method and application.
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.
Flower class Chinese crude drug refers to the medical material be used as medicine with certain part of the flower of plant, inflorescence and flower.Flower class Chinese medicine is indispensable important component part in Chinese material medicine resource, flower apoplexy due to endogenous wind crude drug source enriches, potency range is distributed more widely, wherein the highest with heat clearing away, antidote proportion, is then removing heat from blood, hemorrhage successively, medicine for the treatment of cough and asthma, blood circulation promoting and blood stasis dispelling, wind-expelling pain-stopping medicine, stomach invigorating and Chinese medicine, removing toxic substances diarrhea, Calming liver to disperse Qi decoction, adjusting meridian and stopping leukorrhea medicine etc.The most drug effect of flower class Chinese medicine is gentle, and 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 flower class Chinese crude drug complex chemical composition, traditional extraction process also 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 colored 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 preparation method spending class Chinese crude drug to exempt from decoct, comprises the following steps:
1) flower 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 120 ~ 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) adding its volume 10 ~ 15 times amount volume fraction in the medicinal residues obtained in step 3) is the alcoholic solution of 60% ~ 80%, soaks 30 ~ 60min, then carries out ultrasonic Treatment, filters, obtains filtrate and filtering residue;
5) add the water of its volume 15 ~ 20 times amount in the filtering residue obtained in step 4), soak 60 ~ 120min, then put into microwave and ultrasonic wave synergic extraction instrument and extract, obtain extracting solution;
6) extracting solution that the filtrate that extract step 3) obtained, step 4) obtain, step 5) obtain merges, and then carries out microfiltration, obtains filtrate, filtrate is carried out cryogenic vacuum and concentrates, obtain concentrated solution;
7) concentrated solution spraying dry step 6) obtained, obtains spray drying powder, by spray drying powder nanometer collider pulverizing, obtains nanoscale Chinese medicine microgranule, packs and obtain free decoction agent.
Preferably, supercritical CO in described step 3)
2extraction conditions is: temperature 40 ~ 55 DEG C, pressure 25 ~ 35MPa, CO
2flow velocity 10 ~ 15L/min, extraction time 1.5 ~ 2.5h.
Preferably, in described step 4), supersonic treatment condition is: supersonic frequency 20 ~ 30kHz, power 300 ~ 500W, time 30 ~ 60min, and number of repetition is 2 ~ 3 times.
Preferably, in described step 5), microwave and ultrasonic wave synergic extraction process conditions are: microwave power 300 ~ 500W, time 1 ~ 6min, temperature 40 ~ 60 DEG C, and number of repetition is 2 ~ 3 times.
Preferably, in described step 6), microfiltration process conditions are: filter sizes 0.2 ~ 0.8 μm, operation pressure reduction 0.10 ~ 0.20MPa.
Preferably, concentrated in described step 6) is that filtrate is carried out vacuum concentration 40 ~ 60 DEG C time, and vacuum is 0.08 ~ 0.09MPa, is concentrated into 15% ~ 20% of former filtrate volume.
Preferably, in described step 7), the particle diameter of nanoscale Chinese medicine microgranule is 50 ~ 100nm.
Present invention also offers above-mentioned preparation method gained and exempt from the application of decoct in preparation compound Chinese medicinal preparation, flower 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 flower class active ingredients from traditional Chinese medicinal.First supercritical CO is adopted
2abstraction technique extracts the volatile oil component contained by flower 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 adopt fat-soluble effective ingredient in alcoholic solution Soakage extraction medical material, 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; Finally adopt microwave and ultrasonic wave synergic extraction technology to extract in medical material and remain effective ingredient, microwave and ultrasonic wave synergic extraction technology can improve drug-eluting speed and stripping number of times, and shorten extraction time, selectivity is good, and extracts active ingredients efficiency is high.
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, alcohol extraction are in conjunction with the combination of ultrasonic assistant extraction, microwave and ultrasonic wave synergic extraction technology, 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 flower class Chinese crude drug obtains and effectively extracts and protection, improves the availability of colored class Chinese crude drug.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further elaborated.
Spend class Chinese crude drug to exempt from a preparation method for decoct, comprise the following steps:
1) flower 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 120 ~ 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) adding its volume 10 ~ 15 times amount volume fraction in the medicinal residues obtained in step 3) is the alcoholic solution of 60% ~ 80%, soaks 30 ~ 60min, then carries out ultrasonic Treatment, filters, obtains filtrate and filtering residue;
5) add the water of its volume 15 ~ 20 times amount in the filtering residue obtained in step 4), soak 60 ~ 120min, then put into microwave and ultrasonic wave synergic extraction instrument and extract, obtain extracting solution;
6) extracting solution that the filtrate that extract step 3) obtained, step 4) obtain, step 5) obtain merges, and then carries out microfiltration, obtains filtrate, filtrate is carried out cryogenic vacuum and concentrates, obtain concentrated solution;
7) concentrated solution spraying dry step 6) obtained, obtains spray drying powder, by spray drying powder nanometer collider pulverizing, 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 flower class Chinese crude drug below 3.0% after drying with moisture test apparatus.
In step 2) in, sporoderm-broken rate >=95% of rear crude drug cell pulverized by described super micron mill, and powder diameter is little, is evenly distributed, and specific surface area significantly improves, and dissolving and the release of effective ingredient are accelerated.
In step 3), described supercritical CO
2extraction conditions is preferably: temperature 40 ~ 55 DEG C, pressure 25 ~ 35MPa, CO
2flow velocity 10 ~ 15L/min, extraction time 1.5 ~ 2.5h, 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 supersonic treatment condition is preferably: supersonic frequency 20 ~ 30kHz, power 300 ~ 500W, time 30 ~ 60min, number of repetition is 2 ~ 3 times, and ultrasonic assistant extracts can increase molecular motion of material frequency and speed, increases solvent penetration power, improve drug-eluting speed and stripping number of times, shorten extraction time.
In step 5), described microwave and ultrasonic wave synergic extraction process conditions are preferably: microwave power 300 ~ 500W, time 1 ~ 6min, temperature 40 ~ 60 DEG C, number of repetition is 2 ~ 3 times, microwave and ultrasonic wave synergic extraction technology both can utilize the heating effect ruptured cell of microwave and its electromagnetic field activation effect to accelerate effective ingredient diffusion rate, ultrasound wave can be utilized again to increase molecular motion of material frequency and speed, increase solvent penetration power, improve drug-eluting speed and stripping number of times, extraction rate is faster, and extraction time is shorter, and effective ingredient yield is higher.
In step 6), described microfiltration process conditions are preferably: filter sizes 0.2 ~ 0.8 μm, operation pressure reduction 0.10 ~ 0.20MPa, 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.Described concentrated be that filtrate is carried out vacuum concentration 40 ~ 60 DEG C time, vacuum is 0.08 ~ 0.09MPa, be concentrated into 15% ~ 20% of former filtrate volume, cryogenic vacuum is concentrated can reduce solvent boiling point, temperature is low, speed is fast, the thermal sensitivity effective ingredient in Chinese crude drug can be prevented to be destroyed, to save the effective ingredient of Chinese medicine extraction liquid better.
In step 7), the particle diameter of described nanoscale Chinese medicine microgranule is 50 ~ 100nm.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, flower 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 Flos Magnoliae, it exempts from the preparation method of decoct, comprises the following steps:
1) Flos Magnoliae is picked up clean roguing, carry out cold drying under vacuum;
2) dried Flos Magnoliae super micron mill is ground into the Flos Magnoliae fine powder that particle diameter is 120 ~ 150 μm;
3) by step 2) the Flos Magnoliae fine powder that obtains puts into supercritical CO
2extract in extraction equipment, extraction temperature is 40 DEG C, pressure 25MPa, CO
2flow velocity 10L/min, extraction time 1.5h, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) adding its volume 10 times amount volume fraction in the medicinal residues obtained in step 3) is the alcoholic solution of 60%, soaks 30min, then carries out ultrasonic Treatment, supersonic frequency 20kHz, power 300W, time 30min, repeats 2 times, and filtration, obtains filtrate and filtering residue;
5) add the water of its volume 15 times amount in the filtering residue obtained in step 4), soak 60min, then put into microwave and ultrasonic wave synergic extraction instrument and extract, power 300W, time 1min, temperature 40 DEG C, repeat 2 times, obtain extracting solution;
6) extracting solution that the filtrate that extract step 3) obtained, step 4) obtain, step 5) obtain merges, then microfiltration is carried out with the filter membrane that aperture is 0.2 μm, operation pressure reduction 0.10MPa, obtain filtrate, filtrate is carried out vacuum concentration 40 DEG C time, vacuum is 0.08MPa, is concentrated into 15% of former filtrate volume, obtains concentrated solution;
7) concentrated solution spraying dry step 6) obtained, obtains spray drying powder, by spray drying powder nanometer collider pulverizing, obtains the nanoscale Chinese medicine microgranule that particle diameter is 50 ~ 100nm, packs and obtain free decoction agent.
Embodiment 2
For Flos Sophorae, it exempts from the preparation method of decoct, comprises the following steps:
1) Flos Sophorae is picked up clean roguing, carry out cold drying under vacuum;
2) dried Flos Sophorae super micron mill is ground into the Flos Sophorae fine powder that particle diameter is 120 ~ 150 μm;
3) by step 2) the Flos Sophorae fine powder that obtains puts into supercritical CO
2extract in extraction equipment, extraction temperature is 42 DEG C, pressure 27MPa, CO
2flow velocity 12L/min, extraction time 2h, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) adding its volume 12 times amount volume fraction in the medicinal residues obtained in step 3) is the alcoholic solution of 65%, soaks 40min, then carries out ultrasonic Treatment, supersonic frequency 22kHz, power 350W, time 35min, repeats 2 times, and filtration, obtains filtrate and filtering residue;
5) add the water of its volume 17 times amount in the filtering residue obtained in step 4), soak 70min, then put into microwave and ultrasonic wave synergic extraction instrument and extract, power 350W, time 2min, temperature 42 DEG C, repeat 3 times, obtain extracting solution;
6) extracting solution that the filtrate that extract step 3) obtained, step 4) obtain, step 5) obtain merges, then microfiltration is carried out with the filter membrane that aperture is 0.4 μm, operation pressure reduction 0.12MPa, obtain filtrate, filtrate is carried out vacuum concentration 42 DEG C time, vacuum is 0.085MPa, is concentrated into 16% of former filtrate volume, obtains concentrated solution;
7) concentrated solution spraying dry step 6) obtained, obtains spray drying powder, by spray drying powder nanometer collider pulverizing, obtains the nanoscale Chinese medicine microgranule that particle diameter is 50 ~ 100nm, packs and obtain free decoction agent.
Embodiment 3
For Flos Magnoliae Officinalis, it exempts from the preparation method of decoct, comprises the following steps:
1) Flos Magnoliae Officinalis is picked up clean roguing, carry out cold drying under vacuum;
2) dried Flos Magnoliae Officinalis super micron mill is ground into the Flos Magnoliae Officinalis fine powder that particle diameter is 120 ~ 150 μm;
3) by step 2) the Flos Magnoliae Officinalis fine powder that obtains puts into supercritical CO
2extract in extraction equipment, extraction temperature is 48 DEG C, pressure 30MPa, CO
2flow velocity 13L/min, extraction time 1.8h, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) adding its volume 13 times amount volume fraction in the medicinal residues obtained in step 3) is the alcoholic solution of 70%, soaks 45min, then carries out ultrasonic Treatment, supersonic frequency 25kHz, power 400W, time 45min, repeats 2 times, and filtration, obtains filtrate and filtering residue;
5) add the water of its volume 18 times amount in the filtering residue obtained in step 4), soak 90min, then put into microwave and ultrasonic wave synergic extraction instrument and extract, power 400W, time 3min, temperature 48 DEG C, repeat 2 times, obtain extracting solution;
6) extracting solution that the filtrate that extract step 3) obtained, step 4) obtain, step 5) obtain merges, then microfiltration is carried out with the filter membrane that aperture is 0.6 μm, operation pressure reduction 0.15MPa, obtain filtrate, filtrate is carried out vacuum concentration 48 DEG C time, vacuum is 0.08MPa, is concentrated into 18% of former filtrate volume, obtains concentrated solution;
7) concentrated solution spraying dry step 6) obtained, obtains spray drying powder, by spray drying powder nanometer collider pulverizing, obtains the nanoscale Chinese medicine microgranule that particle diameter is 50 ~ 100nm, packs and obtain free decoction agent.
Embodiment 4
For Flos Carthami, it exempts from the preparation method of decoct, comprises the following steps:
1) Flos Carthami is picked up clean roguing, carry out cold drying under vacuum;
2) dried Flos Carthami super micron mill is ground into the Flos Carthami fine powder that particle diameter is 120 ~ 150 μm;
3) by step 2) the Flos Carthami fine powder that obtains puts into supercritical CO
2extract in extraction equipment, extraction temperature is 50 DEG C, pressure 32MPa, CO
2flow velocity 14L/min, extraction time 2.3h, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) adding its volume 14 times amount volume fraction in the medicinal residues obtained in step 3) is the alcoholic solution of 75%, soaks 50min, then carries out ultrasonic Treatment, supersonic frequency 28kHz, power 450W, time 50min, repeats 3 times, and filtration, obtains filtrate and filtering residue;
5) add the water of its volume 19 times amount in the filtering residue obtained in step 4), soak 100min, then put into microwave and ultrasonic wave synergic extraction instrument and extract, power 450W, time 4min, temperature 50 C, repeat 2 times, obtain extracting solution;
6) extracting solution that the filtrate that extract step 3) obtained, step 4) obtain, step 5) obtain merges, then microfiltration is carried out with the filter membrane that aperture is 0.5 μm, operation pressure reduction 0.18MPa, obtain filtrate, filtrate is carried out vacuum concentration 55 DEG C time, vacuum is 0.09MPa, is concentrated into 19% of former filtrate volume, obtains concentrated solution;
7) concentrated solution spraying dry step 6) obtained, obtains spray drying powder, by spray drying powder nanometer collider pulverizing, obtains the nanoscale Chinese medicine microgranule that particle diameter is 50 ~ 100nm, packs and obtain free decoction agent.
Embodiment 5
For Flos Lonicerae, it exempts from the preparation method of decoct, comprises the following steps:
1) Flos Lonicerae is picked up clean roguing, carry out cold drying under vacuum;
2) dried Flos Lonicerae super micron mill is ground into the Flos Lonicerae fine powder that particle diameter is 120 ~ 150 μm;
3) by step 2) the Flos Lonicerae fine powder that obtains puts into supercritical CO
2extract in extraction equipment, extraction temperature is 55 DEG C, pressure 35MPa, CO
2flow velocity 15L/min, extraction time 2.5h, enter separating still subsequently and be separated, obtain extract and medicinal residues;
4) adding its volume 15 times amount volume fraction in the medicinal residues obtained in step 3) is the alcoholic solution of 80%, soaks 60min, then carries out ultrasonic Treatment, supersonic frequency 30kHz, power 500W, time 60min, repeats 3 times, and filtration, obtains filtrate and filtering residue;
5) add the water of its volume 20 times amount in the filtering residue obtained in step 4), soak 120min, then put into microwave and ultrasonic wave synergic extraction instrument and extract, power 500W, time 6min, temperature 60 C, repeat 3 times, obtain extracting solution;
6) extracting solution that the filtrate that extract step 3) obtained, step 4) obtain, step 5) obtain merges, then microfiltration is carried out with the filter membrane that aperture is 0.8 μm, operation pressure reduction 0.20MPa, obtain filtrate, filtrate is carried out vacuum concentration 60 DEG C time, vacuum is 0.09MPa, is concentrated into 20% of former filtrate volume, obtains concentrated solution;
7) concentrated solution spraying dry step 6) obtained, obtains spray drying powder, by spray drying powder nanometer collider pulverizing, obtains the nanoscale Chinese medicine microgranule that particle diameter is 50 ~ 100nm, packs and obtain free decoction agent.
Below by experiment embodiment, beneficial effect of the present invention is described.
Drug efficacy study
1, to treat the oral traditional Chinese medicine decoction of hyperlipidemia
Chinese medicine formula: Radix Et Rhizoma Rhei 5 parts, Semen Cassiae 10 parts, Pollen Typhae 30 parts, Fructus Ligustri Lucidi 30 parts, 30 parts, Fructus Mori.
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 Radix Et Rhizoma Rhei 5 parts, Semen Cassiae 10 parts, Fructus Ligustri Lucidi 30 parts, 30 parts, Fructus Mori add in Decocting pot to decoct and make decoction; Exempt from spend class Chinese crude drug Pollen Typhae 30 parts to make in formula 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 II.
The inventive method 2: get Radix Et Rhizoma Rhei 5 parts, Semen Cassiae 10 parts, Fructus Ligustri Lucidi 30 parts, Fructus Mori 30 parts of parts add in Decocting pot to decoct and make decoction; Flower class Chinese crude drug consumption in formula is reduced to Pollen Typhae 28 parts of parts, 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 hyperlipemic 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, continuous 30 days courses for the treatment of, a course for the treatment of of light-duty hyperlipidemia, two courses for the treatment of of heavy hyperlipidemia.
Efficacy assessment standard: effective: light, heavy hyperlipidemia this disease symptoms of patient after treatment disappears, and body recovers normal, through laboratory examination, in blood fat normal value, follows up a case by regular visits to l ~ 3 year without recidivist; Take a turn for the better: hyperlipidemic conditions progressively alleviates or disappears, and patient feels good, and body constitution recovers normal substantially; Invalid: not reach improvement standard person.
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 colored 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 chronic pharyngitis
Chinese medicine formula: Fructus Momordicae 10 parts, Radix Pseudostellariae 30 parts, Radix Codonopsis 15 parts, Semen Sterculiae Lychnophorae 10 parts, Semen Oroxyli 6 parts, Pericarpium Citri Reticulatae 10 parts, Fructus Mume 6 parts, 6 parts, Radix Glycyrrhizae, Fructus Canarii albi 10 parts, 10 parts, Herba Passiflorae Caeruleae stem, Ramulus Luffae 20 parts, the Radix Astragali 30 parts, Herba Equiseti Hiemalis 12 parts, Flos Lonicerae 10 parts, the lotus base of a fruit 8 parts, Flos Trollii 6 parts, Fructus Atriplicis Sibiricae 12 parts, Flos Magnoliae 10 parts, dragon well green tea 10 parts.
Contrast method: 1) get it filled by formula, decocts with water secondary, 2 hours first times, second time 1.5 hours, and gradation filters, and merging filtrate, dusts with spray dryer, for subsequent use; 2) dry powder in step 1) is added starch, anhydrous glucose, stevioside, mix homogeneously; 3) said mixture is added 80% ethanol soft material; 4) granulate with soft material 14 mesh sieve, namely granulate obtains granule I.
The inventive method 1: get it filled by formula, is first prepared into flower class Chinese crude drug Flos Lonicerae 10 parts, Flos Trollii 6 parts, Flos Magnoliae 10 parts in formula according to the inventive method and exempts from decoct (concrete grammar is with embodiment 1); Carry out process according to contrast method step 1) obtain dry powder by remaining medical material in formula, dry powder and this method gained are exempted from decoct mixing, add starch, anhydrous glucose, stevioside, mix homogeneously; Mixture is processed according to contrast method step 3) and step 4), obtains granule II.
The inventive method 2: flower class Chinese crude drug consumption in formula is reduced to Flos Lonicerae 8 parts, Flos Trollii 5 parts, Flos Magnoliae 8 parts, is prepared into according to the inventive method and exempts from decoct (concrete grammar is with embodiment 1); Residue medical material is got it filled by formula consumption, carries out process obtain dry powder according to contrast method step 1), dry powder and this method gained is exempted from decoct mixing, adds starch, anhydrous glucose, stevioside, mix homogeneously; Mixture is processed according to contrast method step 3) and step 4), obtains granule III.
Lanqin oral solutions:
Choose 180 routine patients with chronic pharyngitis, the age is between 16 ~ 60 years old.
Above-mentioned 180 routine patients are divided into 3 groups at random, and often organizing 60 examples and take granule I (matched group), granule II (experimental group 1) and granule III (experimental group 2) by same dose respectively, continuous 15 days is a course for the treatment of.
Curative effect determinate standard: recovery from illness: within 10 days, symptom alleviates, within 3 months, clinical symptoms and sign disappear, and within more than 1 year, without recurrence, check that red swelling of the pharynx disappears, pharynx rear wall lymph follicle recovers normal; Effective: within two weeks, symptom alleviates, within 3 months, clinical symptoms and sign disappear, and pharyngeal hyperemia alleviates, but curative effect is not consolidated, and accidental cause Changes in weather speaks that too much flue dust stimulates and symptom slightly recurs, and namely short-term medication heals; Take a turn for the better: within two weeks, symptom alleviates, within 3 months, clinical symptoms and part sign disappear.Irritable cough reduces, and checks that the pharyngeal inflammation that still has changes; Invalid: after medication, symptom slightly alleviates or do not alleviate, and sign is not improved.
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 colored 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, colored 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 (9)
1. spend class Chinese crude drug to exempt from a preparation method for decoct, it is characterized in that, comprise the following steps:
1) flower 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 120 ~ 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) adding its volume 10 ~ 15 times amount volume fraction in the medicinal residues obtained in step 3) is the alcoholic solution of 60% ~ 80%, soaks 30 ~ 60min, then carries out ultrasonic Treatment, filters, obtains filtrate and filtering residue;
5) add the water of its volume 15 ~ 20 times amount in the filtering residue obtained in step 4), soak 60 ~ 120min, then put into microwave and ultrasonic wave synergic extraction instrument and extract, obtain extracting solution;
6) extracting solution that the filtrate that extract step 3) obtained, step 4) obtain, step 5) obtain merges, and then carries out microfiltration, obtains filtrate, filtrate is carried out cryogenic vacuum and concentrates, obtain concentrated solution;
7) concentrated solution spraying dry step 6) obtained, obtains spray drying powder, by spray drying powder nanometer collider pulverizing, obtains nanoscale Chinese medicine microgranule, packs and obtain free decoction agent.
2. a kind of preparation method spending class Chinese crude drug to exempt from decoct as claimed in claim 1, is characterized in that: supercritical CO in described step 3)
2extraction conditions is: temperature 40 ~ 55 DEG C, pressure 25 ~ 35MPa, CO
2flow velocity 10 ~ 15L/min, extraction time 1.5 ~ 2.5h.
3. a kind of preparation method spending class Chinese crude drug to exempt from decoct as claimed in claim 1, it is characterized in that: in described step 4), supersonic treatment condition is: supersonic frequency 20 ~ 30kHz, power 300 ~ 500W, time 30 ~ 60min, number of repetition is 2 ~ 3 times.
4. a kind of preparation method spending class Chinese crude drug to exempt from decoct as claimed in claim 1, it is characterized in that: in described step 5), microwave and ultrasonic wave synergic extraction process conditions are: microwave power 300 ~ 500W, time 1 ~ 6min, temperature 40 ~ 60 DEG C, number of repetition is 2 ~ 3 times.
5. a kind of preparation method spending class Chinese crude drug to exempt from decoct as claimed in claim 1, is characterized in that: in described step 6), microfiltration process conditions are: filter sizes 0.2 ~ 0.8 μm, operation pressure reduction 0.10 ~ 0.20MPa.
6. a kind of preparation method spending class Chinese crude drug to exempt from decoct as claimed in claim 1, is characterized in that: concentrated in described step 6) is that filtrate is carried out vacuum concentration 40 ~ 60 DEG C time, and vacuum is 0.08 ~ 0.09MPa, is concentrated into 15% ~ 20% of former filtrate volume.
7. a kind of preparation method spending class Chinese crude drug to exempt from decoct as claimed in claim 1, is characterized in that: in described step 7), the particle diameter of nanoscale Chinese medicine microgranule is 50 ~ 100nm.
8. the colored class Chinese crude drug as described in any one of claim 1 ~ 7 exempts from the application of decoct in preparation compound Chinese medicinal preparation, it is characterized in that: flower class Chinese crude drug is exempted from decoct and directly adds in compound Chinese medicinal preparation, make pharmaceutically useful dosage form.
9. flower class Chinese crude drug as claimed in claim 8 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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| CN105707888A (en) * | 2016-03-07 | 2016-06-29 | 河南省南山菇业有限公司 | Nutritious oatmeal capable of clearing away heat and toxic materials and preparation method thereof |
| CN105707702A (en) * | 2016-03-07 | 2016-06-29 | 河南省南山菇业有限公司 | Oatmeal for regulating qi and blood and preparation method thereof |
| CN111074396A (en) * | 2019-12-19 | 2020-04-28 | 界首市华宇纺织有限公司 | Preparation method of antibacterial and deodorant pearl antibacterial yarn |
| RU2810497C1 (en) * | 2022-10-21 | 2023-12-27 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Восточно-Сибирский государственный университет технологий и управления" | Method of obtaining plant extracts |
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| CN102949526A (en) * | 2012-11-29 | 2013-03-06 | 西安福安创意咨询有限责任公司 | Healthcare particles for treating chronic pharyngitis and preparation method thereof |
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| CN101822697A (en) * | 2009-07-13 | 2010-09-08 | 湖南省中医药研究院 | Preparation method of traditional Chinese medicine ultrafine formula particles |
| CN102670869A (en) * | 2012-06-04 | 2012-09-19 | 黄芸 | Chinese medicine oral fluid containing cattail pollen for relieving hyperlipoidemia and preparing method thereof |
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| CN105707888A (en) * | 2016-03-07 | 2016-06-29 | 河南省南山菇业有限公司 | Nutritious oatmeal capable of clearing away heat and toxic materials and preparation method thereof |
| CN105707702A (en) * | 2016-03-07 | 2016-06-29 | 河南省南山菇业有限公司 | Oatmeal for regulating qi and blood and preparation method thereof |
| CN111074396A (en) * | 2019-12-19 | 2020-04-28 | 界首市华宇纺织有限公司 | Preparation method of antibacterial and deodorant pearl antibacterial yarn |
| RU2810497C1 (en) * | 2022-10-21 | 2023-12-27 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Восточно-Сибирский государственный университет технологий и управления" | Method of obtaining plant extracts |
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Application publication date: 20151209 |