CN103800884A - Method for preparing snake gall and dried tangerine peel oral solution - Google Patents
Method for preparing snake gall and dried tangerine peel oral solution Download PDFInfo
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- CN103800884A CN103800884A CN201410062892.8A CN201410062892A CN103800884A CN 103800884 A CN103800884 A CN 103800884A CN 201410062892 A CN201410062892 A CN 201410062892A CN 103800884 A CN103800884 A CN 103800884A
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Abstract
The invention relates to a method for preparing a traditional Chinese medicinal preparation namely a snake gall and dried tangerine peel oral solution, in particular relates to a new method for preparing the snake gall and dried tangerine peel oral solution, and belongs to the technical field of medicines. According to the method for preparing the snake gall and dried tangerine peel oral solution, dried tangerine peel is subjected to supercritical fluid extraction, decoction dregs are subjected to ethanol microwave extraction, and snake gall juice is added to prepare the oral solution.
Description
Technical field
The present invention relates to field of traditional Chinese medicine pharmacy, be specifically related to a kind of preparation method of the SHEDAN CHENPI KOUFUYE with the pleasant stomach strengthening function that reduces phlegm, dispels the wind, belong to medical technical field.
Background technology
Compound recipe SHEDAN CHENPI KOUFUYE is a kind of Chinese patent medicine (compound Chinese medicinal preparation) of the pleasant stomach invigorating of reducing phlegm, dispel the wind, and has applied for many years in China, and clinical in diseases such as cough due to wind and cold, abundant expectoration vomiting, curative effect is sure.SHEDAN CHENPI KOUFUYE is by Chinese medicine Fel Serpentis, the oral liquid of Pericarpium Citri Reticulatae (steaming) through being processed into.This standard is recorded in become a full member the 5th, standard Chinese medicine of Drug Standard of Ministry of Public Health of the Peoples Republic of China new drug, standard No. WS3-104-(Z-17)-94(Z).The technology features of existing Chinese medicine preparation preserved snake gall orange peel powder is that Pericarpium Citri Reticulatae is ground into fine powder, mixes with Fel Serpentis, dry, pulverize, and sieves, and to obtain final product.This processing step is coarse, and the former powder of Pericarpium Citri Reticulatae is used as medicine increases dose, it is slow to absorb, bioavailability is low, quality is wayward.
ZL200810107352.1 discloses a kind of preparation method of SHEDAN CHENPI KOUFUYE, and Fel Serpentis duds is got bile, adds appropriate ethanol, staticly settles, and gets supernatant and reclaims ethanol; Pericarpium Citri Reticulatae decocting boils ethanol precipitation, collects Rhizoma Zingiberis Recens and Semen Armeniacae Amarum distillate, then adds appropriate amount of auxiliary materials and prepare oral liquid.ZL201210128361.5 discloses a kind of preparation method of SHEDAN CHENPI KOUFUYE equally, Pericarpium Citri Reticulatae ethanol extraction, and aqueous alkali acidify postprecipitation, filters and adds Fel Serpentis and adjuvant to prepare oral liquid.The problems such as above-mentioned preparation method all exists extracts active ingredients insufficient, absorbs slowly, and bioavailability is low, and clarity, stability are low need to be overcome.
The present invention, through research, provides a kind of new SHEDAN CHENPI KOUFUYE preparation method, and has found the optimal proportion of Fel Serpentis and Pericarpium Citri Reticulatae, to improve drug effect, overcomes the problems such as in prior art, this product bioavailability is low, preparation is unstable.
Summary of the invention
The object of this invention is to provide a kind of preparation method of the SHEDAN CHENPI KOUFUYE with the pleasant digestion promoting function that reduces phlegm, dispels the wind.
The object of the invention is to implement by following technical proposal:
A kind of preparation method of SHEDAN CHENPI KOUFUYE:
Wherein, the weight portion of selecting crude drug is 7-9 parts of Fel Serpentis, 95-105 parts of Pericarpium Citri Reticulataes, 10-15 parts, Rhizoma Zingiberis Recens, 25-35 parts, Semen Armeniacae Amarum;
(1) take by weight Pericarpium Citri Reticulatae, in CO
2in supercritical extraction reactor, extract volatile oil, wherein pressure is 15-25Mpa, and extraction kettle temperature is 45-55 ℃, CO
2flow velocity is 15-25L/h, and extraction time is 1.0-2.5 hours, collects Pericarpium Citri Reticulatae volatile oil (I) for subsequent use; The ethanol microwave extracting that residue medicinal residues are 75-85% by the concentration of 5-7 times of amounts 1-2 times, each 15-40min, microwave extracting power 450-550W, 50-70 ℃ of temperature, combining extraction liquid, filters, and reclaims ethanol extremely without alcohol taste, add the hot water of 2 times of consumptions of crude drug, slowly add stirring and dissolving, staticly settle, filter and remove precipitation, be concentrated into relative density and be 1.05-1.15 clear paste I, for subsequent use;
(2) get Pericarpium Citri Reticulatae volatile oil with a small amount of dissolve with ethanol, separately get the hydroxypropyl beta-cyclodextrin of 20-30 times of amounts of volatile oil total amount, add the water of 3-6 times of amounts of hydroxypropyl beta-cyclodextrin weight to grind well, add therein again the dissolve with ethanol liquid of Pericarpium Citri Reticulatae volatile oil, grind to form pasty state, after cold drying, obtain Pericarpium Citri Reticulatae volatile oil clathrate with alcoholic solution cleaning, drying;
(3) Rhizoma Zingiberis Recens section adds water to distill and collects distillate, and Semen Armeniacae Amarum adds water to distill and collects distillate, for subsequent use;
(4) qinghuo reagent I adds Fel Serpentis, Pericarpium Citri Reticulatae volatile oil clathrate, Semen Armeniacae Amarum distilled water, Rhizoma Zingiberis Recens distilled water to merge to stir, then adds that Flos Chrysanthemi is sweet, sorbic acid is appropriate, and mix homogeneously, filters embedding, sterilizing.
Preferred technical scheme is:
A kind of preparation method of SHEDAN CHENPI KOUFUYE:
Wherein, the weight portion of selecting crude drug is 8.6 parts of Fel Serpentis, 100 parts of Pericarpium Citri Reticulataes, 12 parts, Rhizoma Zingiberis Recens, 30 parts, Semen Armeniacae Amarum;
(1) take by weight Pericarpium Citri Reticulatae, in CO
2in supercritical extraction reactor, extract volatile oil, wherein pressure is 20Mpa, and extraction kettle temperature is 45 ℃, CO
2flow velocity is 20L/h, and extraction time is 2 hours, collects Pericarpium Citri Reticulatae volatile oil (I) for subsequent use; The ethanol microwave extracting that residue medicinal residues are 80% by the concentration of 7 times of amounts 2 times, each 30min, microwave extracting power 500W, temperature 70 C, combining extraction liquid, filters, and reclaims ethanol extremely without alcohol taste, add the hot water of 2 times of consumptions of crude drug, slowly add stirring and dissolving, staticly settle, filter and remove precipitation, be concentrated into relative density and be 1.10 clear paste I, for subsequent use;
(2) get Pericarpium Citri Reticulatae volatile oil with a small amount of dissolve with ethanol, separately get the hydroxypropyl beta-cyclodextrin of 24 times of amounts of volatile oil total amount, add the water of 3 times of amounts of hydroxypropyl beta-cyclodextrin weight to grind well, add therein again the dissolve with ethanol liquid of Pericarpium Citri Reticulatae volatile oil, grind to form pasty state, after cold drying, obtain Pericarpium Citri Reticulatae volatile oil clathrate with alcoholic solution cleaning, drying;
(3) Rhizoma Zingiberis Recens section adds water to distill and collects distillate, and Semen Armeniacae Amarum adds water to distill and collects distillate, for subsequent use;
(4) qinghuo reagent I adds Fel Serpentis, Pericarpium Citri Reticulatae volatile oil clathrate, Semen Armeniacae Amarum distilled water, Rhizoma Zingiberis Recens distilled water to merge to stir, then adds that Flos Chrysanthemi is sweet, sorbic acid is appropriate, and mix homogeneously, filters embedding, sterilizing.
SHEDAN CHENPI KOUFUYE preparation method of the present invention has following beneficial effect:
1. the processing step in pair standard carries out process modification, extracts Pericarpium Citri Reticulatae crude drug effective ingredient, reduces the content of beary metal such as arsenic salt, improves preparation stability.
2. first Pericarpium Citri Reticulatae volatile oil is carried out to supercritical extraction, and with cyclodextrin inclusion compound, again medicinal residues are carried out to ethanol extraction, not only take full advantage of the Hesperidin effective constituents in Pericarpium Citri Reticulatae, equally another kind of important effective ingredient volatile oil in Pericarpium Citri Reticulatae is collected and is used as medicine, avoid boiling or the loss of ethanol extraction to volatile oil through decocting, improve bioavailability.
3. the optimum amount proportioning that Fel Serpentis and Pericarpium Citri Reticulatae are provided, gives full play to drug effect.
SHEDAN CHENPI KOUFUYE of the present invention is natural medicine, has effect of the pleasant spleen invigorating of reducing phlegm, dispel the wind, is mainly used in treating turbid phlegm obstructing in the lung, stomach-QI being unable to descend normally, cough, vomiting.
The therapeutic effect of the SHEDAN CHENPI KOUFUYE product combining by the improvement of above process conditions improves a lot compared with original product, and stability also improves relatively.
To Pericarpium Citri Reticulatae microwave extraction process conditional filtering step, experiment is given an example below:
1. the selection of extracting method
Take content of hesperidin as index, extract Hesperidin in Pericarpium Citri Reticulatae with different solvents (pure water, ethanol), different modes (microwave and conventional method), determine the optimum extracting method of Pericarpium Citri Reticulatae, experimental establishment and the results are shown in Table 1.
Table 1 different solvents, distinct methods extract Hesperidin experimental result in Pericarpium Citri Reticulatae
| Solvent species | Conventional method (%) | Microwave method (%) |
| Pure water | 1.243 | 1.867 |
| PH8 sodium hydrate aqueous solution | 1.532 | 2.089 |
| 60% ethanol | 1.987 | 2.765 |
Take content of hesperidin as index, from table, result can be found out, the microwave extraction method that extraction solvent is ethanol is the highest compared with other solvents and conventional extracting method gained content of hesperidin, has significant difference.
2. determine Pericarpium Citri Reticulatae microwave extract method by orthogonal experiment
The principal element that affects microwave extraction process has concentration of alcohol, microwave power, extraction temperature and extraction time.Above-mentioned 4 factors are respectively got 3 levels and are carried out L
9(3
4) orthogonal test, get Pericarpium Citri Reticulatae coarse powder 20g, take Hesperidin as evaluation index, screening optimum extraction process, experimental establishment and the results are shown in Table 1
Table 1 factor level table
Take content of hesperidin as index, range analysis result: A>D>B>C.The factor order that affects alcohol extraction effect is concentration of alcohol > extraction temperature > microwave power > extraction time.Optimum process condition is A
2b
2c
3d
3, i.e. 70% ethanol, 500W, extracts 30min, and extracting temperature is 70 ℃.Take C factor as the further variance analysis of error term, concentration of alcohol has appreciable impact to microwave extracting result.
Pharmacodynamic experiment of the present invention
The eliminating the phlegm of this experimentation SHEDAN CHENPI KOUFUYE (new technology) (make by embodiment 2, lower with), antitussive and intestinal advance the effect of several respects, confirm its Pharmacodynamics effect.
1. SHEDAN CHENPI KOUFUYE (new technology) phlegm-dispelling functions test
(1). laboratory animal
ICR mice (male and female half and half)
(2). trial drug
The medicine that embodiment 2 obtains, the SHEDAN CHENPI KOUFUYE (former technique 1) bought on the market (according to the 5th technique of the standard Chinese medicine preparation of becoming a full member of health drug standard new drug promulgated by the ministries or commissions of the Central Government), the preparation method of the disclosed a kind of SHEDAN CHENPI KOUFUYE of former technique 2(ZL200810107352.1), the preparation method of the disclosed a kind of SHEDAN CHENPI KOUFUYE of former technique 3(ZL201210128361.5) respectively obtain medicine.
(3). the foundation of animal model and experimental technique
(3.1) animal grouping
According to the grouping of tested medicine, 10 every group, be set as blank group (0.5 % CMC-Na), the former technique 1 of matched group 1(), the former technique 2 of matched group 2(), the former technique 3 of matched group 3(), tested medicine group (Chinese medicine composition embodiment 2 of the present invention).
(3.2) expectorant test
Mice fasting 20h before experiment, can't help drinking-water, the 1st the sky, each administration in afternoon 1 time, 60min after administration in morning next day, the phenol red normal saline solution 0.7ml of ip.0.25%, after 30min, put to death mice, face upward on a fixing operation plate, cut off skin in neck, separate trachea, under larynx, insert intubate, fix with silk thread ligation, with 5% NaHCO
3rinse, wash altogether 3 times, each 0.5ml, merges 3 times cleaning mixture, adds 50% alcoholic solution to 10ml, and the centrifugal 10min of 3000rpm, in 546nm colorimetric determination optical density.Calculate phenol red concentration according to phenol red standard curve, the results are shown in Table 3.
(3.3) experimental result and analysis
The phlegm-dispelling functions of table 3 SHEDAN CHENPI KOUFUYE
Note: with blank group
#/
##: P<0.01; There is utmost point significant difference
With matched group ratio:
* △ ☆: P<0.05: there is significant difference;
* △ △ ☆ ☆ ##: P<0.01: there is utmost point significant difference
Experimental result shows that SHEDAN CHENPI KOUFUYE that preparation method of the present invention makes can make mice trachea secrete phenol red amount and obviously increase, relatively there were significant differences for phlegm-dispelling functions and matched group, there is better expectorant effect (P < 0.05), and be dose-dependence.
2. SHEDAN CHENPI KOUFUYE (new technology) antitussive effect test
(1). laboratory animal is identical with 1 expectorant test with trial drug;
(2). the foundation of animal model and experimental technique
(2.1) animal grouping is identical with 1 expectorant test
(2.2) antitussive test
The 1st the sky, each administration in afternoon 1 time, 60min after administration in morning next day, is placed in glass bell jar by mice, built-in containing 1 of 0.1ml ammonia cotton balls, observes immediately and record the cough number of times in latent time and the 2min that mice starts to occur cough, the results are shown in Table 4.
(2.3) experimental result and analysis
The antitussive effect of table 4 SHEDAN CHENPI KOUFUYE
Note: with blank group
#/
##: P<0.01; There is utmost point significant difference
With matched group ratio:
* △ ☆: P<0.05: there is significant difference;
* △ △ ☆ ☆: P<0.01: there is utmost point significant difference
Experimental result shows that the SHEDAN CHENPI KOUFUYE that preparation method of the present invention makes can make mouse cough latent time obviously extend, in 2min, cough number of times all has obvious decline, relatively there were significant differences for antitussive effect and matched group, have better antitussive effect (P < 0.05), difference has significant statistical significance.
3. SHEDAN CHENPI KOUFUYE (new technology) promotes gastrointestinal motility test
(1). laboratory animal is identical with 1 expectorant test with trial drug;
(2). the foundation of animal model and experimental technique
(2.1) animal grouping is identical with 1 expectorant test
(2.2) promote gastrointestinal motility
Fasting 20h before experiment.After administration, 60min only gives respectively 10% carbon powder suspension 0.2ml/ respectively, puts to death mice after 20min.The taking-up gastrointestinal of cutting open the belly at once, measures from stomach pylorus to carbon powder Front distance and small intestinal total length (pylorus is to ileocecus), calculates intestinal ink propulsive rate [pylorus is to carbon powder Front distance (cm) ÷ small intestinal total length (cm) * 100%], the results are shown in Table 5.
The promotion gastrointestinal motility result of the test of table 5 SHEDAN CHENPI KOUFUYE
Note: with blank group
#/
##: P<0.01; There is utmost point significant difference
With matched group ratio:
* △ ☆: P<0.05: there is significant difference;
* △ △ ☆ ☆: P<0.01: there is utmost point significant difference
Experimental result shows that the SHEDAN CHENPI KOUFUYE that preparation method of the present invention makes can make mice alvine pushing rate obviously improve, relatively there were significant differences to promote gastrointestinal motility effect and matched group, have better promotion gastrointestinal motility effect (P < 0.05), difference has significant statistical significance.
The specific embodiment
Below in conjunction with embodiment, the present invention is described further.Following examples are only several specific embodiment of the present invention, but design concept of the present invention is not limited to this, allly utilize this design to carry out the change of unsubstantiality to the present invention, all should belong to the behavior of invading protection domain of the present invention.
Embodiment 1
A kind of preparation method of SHEDAN CHENPI KOUFUYE:
Wherein, the weight portion of selecting crude drug is 7 parts of Fel Serpentis, 95 parts of Pericarpium Citri Reticulataes, 10 parts, Rhizoma Zingiberis Recens, 25 parts, Semen Armeniacae Amarum;
(1) take by weight Pericarpium Citri Reticulatae, in CO
2in supercritical extraction reactor, extract volatile oil, wherein pressure is 15Mpa, and extraction kettle temperature is 45 ℃, CO
2flow velocity is 15L/h, and extraction time is 1.0 hours, collects Pericarpium Citri Reticulatae volatile oil (I) for subsequent use; The ethanol microwave extracting that residue medicinal residues are 75 by the concentration of 5 times of amounts 1 time, each 15min, microwave extracting power 450W, temperature 50 C, combining extraction liquid, filters, and reclaims ethanol extremely without alcohol taste, add the hot water of 2 times of consumptions of crude drug, slowly add stirring and dissolving, staticly settle, filter and remove precipitation, be concentrated into relative density and be 1.05 clear paste I, for subsequent use;
(2) get Pericarpium Citri Reticulatae volatile oil with a small amount of dissolve with ethanol, separately get the hydroxypropyl beta-cyclodextrin of 20 times of amounts of volatile oil total amount, add the water of 3 times of amounts of hydroxypropyl beta-cyclodextrin weight to grind well, add therein again the dissolve with ethanol liquid of Pericarpium Citri Reticulatae volatile oil, grind to form pasty state, after cold drying, obtain Pericarpium Citri Reticulatae volatile oil clathrate with alcoholic solution cleaning, drying;
(3) Rhizoma Zingiberis Recens section adds water to distill and collects distillate, and Semen Armeniacae Amarum adds water to distill and collects distillate, for subsequent use;
(4) qinghuo reagent I adds Fel Serpentis, Pericarpium Citri Reticulatae volatile oil clathrate, Semen Armeniacae Amarum distilled water, Rhizoma Zingiberis Recens distilled water to merge to stir, then adds that Flos Chrysanthemi is sweet, sorbic acid is appropriate, and mix homogeneously, filters embedding, sterilizing.
Embodiment 2
A kind of preparation method of SHEDAN CHENPI KOUFUYE:
Wherein, the weight portion of selecting crude drug is 8.6 parts of Fel Serpentis, 100 parts of Pericarpium Citri Reticulataes, 12 parts, Rhizoma Zingiberis Recens, 30 parts, Semen Armeniacae Amarum;
(1) take by weight Pericarpium Citri Reticulatae, in CO
2in supercritical extraction reactor, extract volatile oil, wherein pressure is 20Mpa, and extraction kettle temperature is 45 ℃, CO
2flow velocity is 20L/h, and extraction time is 2 hours, collects Pericarpium Citri Reticulatae volatile oil (I) for subsequent use; The ethanol microwave extracting that residue medicinal residues are 80% by the concentration of 7 times of amounts 2 times, each 30min, microwave extracting power 500W, temperature 70 C, combining extraction liquid, filters, and reclaims ethanol extremely without alcohol taste, add the hot water of 2 times of consumptions of crude drug, slowly add stirring and dissolving, staticly settle, filter and remove precipitation, be concentrated into relative density and be 1.10 clear paste I, for subsequent use;
(2) get Pericarpium Citri Reticulatae volatile oil with a small amount of dissolve with ethanol, separately get the hydroxypropyl beta-cyclodextrin of 24 times of amounts of volatile oil total amount, add the water of 3 times of amounts of hydroxypropyl beta-cyclodextrin weight to grind well, add therein again the dissolve with ethanol liquid of Pericarpium Citri Reticulatae volatile oil, grind to form pasty state, after cold drying, obtain Pericarpium Citri Reticulatae volatile oil clathrate with alcoholic solution cleaning, drying;
(3) Rhizoma Zingiberis Recens section adds water to distill and collects distillate, and Semen Armeniacae Amarum adds water to distill and collects distillate, for subsequent use;
(4) qinghuo reagent I adds Fel Serpentis, Pericarpium Citri Reticulatae volatile oil clathrate, Semen Armeniacae Amarum distilled water, Rhizoma Zingiberis Recens distilled water to merge to stir, then adds that Flos Chrysanthemi is sweet, sorbic acid is appropriate, and mix homogeneously, filters embedding, sterilizing.
Embodiment 3:
A kind of preparation method of SHEDAN CHENPI KOUFUYE:
Wherein, the weight portion of selecting crude drug is 9 parts of Fel Serpentis, 105 parts of Pericarpium Citri Reticulataes, 15 parts, Rhizoma Zingiberis Recens, 35 parts, Semen Armeniacae Amarum;
(1) take by weight Pericarpium Citri Reticulatae, in CO
2in supercritical extraction reactor, extract volatile oil, wherein pressure is 25Mpa, and extraction kettle temperature is 55 ℃, CO
2flow velocity is 25L/h, and extraction time is 2.5 hours, collects Pericarpium Citri Reticulatae volatile oil (I) for subsequent use; The ethanol microwave extracting that residue medicinal residues are 85% by the concentration of 7 times of amounts 2 times, each 40min, microwave extracting power 550W, temperature 70 C, combining extraction liquid, filters, and reclaims ethanol extremely without alcohol taste, add the hot water of 2 times of consumptions of crude drug, slowly add stirring and dissolving, staticly settle, filter and remove precipitation, be concentrated into relative density and be 1.15 clear paste I, for subsequent use;
(2) get Pericarpium Citri Reticulatae volatile oil with a small amount of dissolve with ethanol, separately get the hydroxypropyl beta-cyclodextrin of 30 times of amounts of volatile oil total amount, add the water of 6 times of amounts of hydroxypropyl beta-cyclodextrin weight to grind well, add therein again the dissolve with ethanol liquid of Pericarpium Citri Reticulatae volatile oil, grind to form pasty state, after cold drying, obtain Pericarpium Citri Reticulatae volatile oil clathrate with alcoholic solution cleaning, drying;
(3) Rhizoma Zingiberis Recens section adds water to distill and collects distillate, and Semen Armeniacae Amarum adds water to distill and collects distillate, for subsequent use;
(4) qinghuo reagent I adds Fel Serpentis, Pericarpium Citri Reticulatae volatile oil clathrate, Semen Armeniacae Amarum distilled water, Rhizoma Zingiberis Recens distilled water to merge to stir, then adds that Flos Chrysanthemi is sweet, sorbic acid is appropriate, and mix homogeneously, filters embedding, sterilizing.
Claims (4)
1. a preparation method for SHEDAN CHENPI KOUFUYE, wherein, the weight portion of selecting crude drug is 7-9 parts of Fel Serpentis, 95-105 parts of Pericarpium Citri Reticulataes, 10-15 parts, Rhizoma Zingiberis Recens, 25-35 parts, Semen Armeniacae Amarum;
(1) take by weight Pericarpium Citri Reticulatae, in CO
2in supercritical extraction reactor, extract volatile oil, wherein pressure is 15-25Mpa, and extraction kettle temperature is 45-55 ℃, CO
2flow velocity is 15-25L/h, and extraction time is 1.0-2.5 hours, collects Pericarpium Citri Reticulatae volatile oil (I) for subsequent use; The ethanol microwave extracting that residue medicinal residues are 75-85% by the concentration of 5-7 times of amounts 1-2 times, each 15-40min, microwave extracting power 450-550W, 50-70 ℃ of temperature, combining extraction liquid, filters, and reclaims ethanol extremely without alcohol taste, add the hot water of 2 times of consumptions of crude drug, slowly add stirring and dissolving, staticly settle, filter and remove precipitation, be concentrated into relative density and be 1.05-1.15 clear paste I, for subsequent use;
(2) get Pericarpium Citri Reticulatae volatile oil with a small amount of dissolve with ethanol, separately get the hydroxypropyl beta-cyclodextrin of 20-30 times of amounts of volatile oil total amount, add the water of 3-6 times of amounts of hydroxypropyl beta-cyclodextrin weight to grind well, add therein again the dissolve with ethanol liquid of Pericarpium Citri Reticulatae volatile oil, grind to form pasty state, after cold drying, obtain Pericarpium Citri Reticulatae volatile oil clathrate with alcoholic solution cleaning, drying;
(3) Rhizoma Zingiberis Recens section adds water to distill and collects distillate, and Semen Armeniacae Amarum adds water to distill and collects distillate, for subsequent use;
(4) qinghuo reagent I adds Fel Serpentis, Pericarpium Citri Reticulatae volatile oil clathrate, Semen Armeniacae Amarum distilled water, Rhizoma Zingiberis Recens distilled water to merge to stir, then adds that Flos Chrysanthemi is sweet, sorbic acid is appropriate, and mix homogeneously, filters embedding, sterilizing.
2. the preparation method of a kind of SHEDAN CHENPI KOUFUYE according to claim 1, wherein, the weight portion of selecting crude drug is 8-6 parts of Fel Serpentis, 100 parts of Pericarpium Citri Reticulataes, 12 parts, Rhizoma Zingiberis Recens, 30 parts, Semen Armeniacae Amarum;
(1) take by weight Pericarpium Citri Reticulatae, in CO
2in supercritical extraction reactor, extract volatile oil, wherein pressure is 20Mpa, and extraction kettle temperature is 45 ℃, CO
2flow velocity is 20L/h, and extraction time is 2 hours, collects Pericarpium Citri Reticulatae volatile oil (I) for subsequent use; The ethanol microwave extracting that residue medicinal residues are 80% by the concentration of 7 times of amounts 2 times, each 30min, microwave extracting power 500W, temperature 70 C, combining extraction liquid, filters, and reclaims ethanol extremely without alcohol taste, add the hot water of 2 times of consumptions of crude drug, slowly add stirring and dissolving, staticly settle, filter and remove precipitation, be concentrated into relative density and be 1.10 clear paste I, for subsequent use;
(2) get Pericarpium Citri Reticulatae volatile oil with a small amount of dissolve with ethanol, separately get the hydroxypropyl beta-cyclodextrin of 24 times of amounts of volatile oil total amount, add the water of 3 times of amounts of hydroxypropyl beta-cyclodextrin weight to grind well, add therein again the dissolve with ethanol liquid of Pericarpium Citri Reticulatae volatile oil, grind to form pasty state, after cold drying, obtain Pericarpium Citri Reticulatae volatile oil clathrate with alcoholic solution cleaning, drying;
(3) Rhizoma Zingiberis Recens section adds water to distill and collects distillate, and Semen Armeniacae Amarum adds water to distill and collects distillate, for subsequent use;
(4) qinghuo reagent I adds Fel Serpentis, Pericarpium Citri Reticulatae volatile oil clathrate, Semen Armeniacae Amarum distilled water, Rhizoma Zingiberis Recens distilled water to merge to stir, then adds that Flos Chrysanthemi is sweet, sorbic acid is appropriate, and mix homogeneously, filters embedding, sterilizing.
3. the preparation method of a kind of SHEDAN CHENPI KOUFUYE according to claim 1, wherein, the weight portion of selecting crude drug is 7 parts of Fel Serpentis, 95 parts of Pericarpium Citri Reticulataes, 10 parts, Rhizoma Zingiberis Recens, 25 parts, Semen Armeniacae Amarum;
(1) take by weight Pericarpium Citri Reticulatae, in CO
2in supercritical extraction reactor, extract volatile oil, wherein pressure is 15Mpa, and extraction kettle temperature is 45 ℃, CO
2flow velocity is 15L/h, and extraction time is 1.0 hours, collects Pericarpium Citri Reticulatae volatile oil (I) for subsequent use; The ethanol microwave extracting that residue medicinal residues are 75 by the concentration of 5 times of amounts 1 time, each 15min, microwave extracting power 450W, temperature 50 C, combining extraction liquid, filters, and reclaims ethanol extremely without alcohol taste, add the hot water of 2 times of consumptions of crude drug, slowly add stirring and dissolving, staticly settle, filter and remove precipitation, be concentrated into relative density and be 1.05 clear paste I, for subsequent use;
(2) get Pericarpium Citri Reticulatae volatile oil with a small amount of dissolve with ethanol, separately get the hydroxypropyl beta-cyclodextrin of 20 times of amounts of volatile oil total amount, add the water of 3 times of amounts of hydroxypropyl beta-cyclodextrin weight to grind well, add therein again the dissolve with ethanol liquid of Pericarpium Citri Reticulatae volatile oil, grind to form pasty state, after cold drying, obtain Pericarpium Citri Reticulatae volatile oil clathrate with alcoholic solution cleaning, drying;
(3) Rhizoma Zingiberis Recens section adds water to distill and collects distillate, and Semen Armeniacae Amarum adds water to distill and collects distillate, for subsequent use;
(4) qinghuo reagent I adds Fel Serpentis, Pericarpium Citri Reticulatae volatile oil clathrate, Semen Armeniacae Amarum distilled water, Rhizoma Zingiberis Recens distilled water to merge to stir, then adds that Flos Chrysanthemi is sweet, sorbic acid is appropriate, and mix homogeneously, filters embedding, sterilizing.
4. the preparation method of a kind of SHEDAN CHENPI KOUFUYE according to claim 1, wherein, the weight portion of selecting crude drug is 9 parts of Fel Serpentis, 105 parts of Pericarpium Citri Reticulataes, 15 parts, Rhizoma Zingiberis Recens, 35 parts, Semen Armeniacae Amarum;
(1) take by weight Pericarpium Citri Reticulatae, in CO
2in supercritical extraction reactor, extract volatile oil, wherein pressure is 25Mpa, and extraction kettle temperature is 55 ℃, CO
2flow velocity is 25L/h, and extraction time is 2.5 hours, collects Pericarpium Citri Reticulatae volatile oil (I) for subsequent use; The ethanol microwave extracting that residue medicinal residues are 85% by the concentration of 7 times of amounts 2 times, each 40min, microwave extracting power 550W, temperature 70 C, combining extraction liquid, filters, and reclaims ethanol extremely without alcohol taste, add the hot water of 2 times of consumptions of crude drug, slowly add stirring and dissolving, staticly settle, filter and remove precipitation, be concentrated into relative density and be 1.15 clear paste I, for subsequent use;
(2) get Pericarpium Citri Reticulatae volatile oil with a small amount of dissolve with ethanol, separately get the hydroxypropyl beta-cyclodextrin of 30 times of amounts of volatile oil total amount, add the water of 6 times of amounts of hydroxypropyl beta-cyclodextrin weight to grind well, add therein again the dissolve with ethanol liquid of Pericarpium Citri Reticulatae volatile oil, grind to form pasty state, after cold drying, obtain Pericarpium Citri Reticulatae volatile oil clathrate with alcoholic solution cleaning, drying;
(3) Rhizoma Zingiberis Recens section adds water to distill and collects distillate, and Semen Armeniacae Amarum adds water to distill and collects distillate, for subsequent use;
(4) qinghuo reagent I adds Fel Serpentis, Pericarpium Citri Reticulatae volatile oil clathrate, Semen Armeniacae Amarum distilled water, Rhizoma Zingiberis Recens distilled water to merge to stir, then adds that Flos Chrysanthemi is sweet, sorbic acid is appropriate, and mix homogeneously, filters embedding, sterilizing.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1843440A (en) * | 2006-02-23 | 2006-10-11 | 北京阜康仁生物制药科技有限公司 | Traditional Chinese medicine formulation and its novel preparation method |
| CN101422596A (en) * | 2008-11-07 | 2009-05-06 | 江西昌诺药业有限公司 | Preserved snake gall orange peel oral liquid and quality control method thereof |
| CN102552806A (en) * | 2012-01-10 | 2012-07-11 | 山东中医药大学附属医院 | Fat-burning dredging particles and preparation method thereof |
| CN103372081A (en) * | 2012-04-27 | 2013-10-30 | 江西济民可信药业有限公司 | Preparation method of Chinese herba preparation snake gall-dried orange peel oral liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1843440A (en) * | 2006-02-23 | 2006-10-11 | 北京阜康仁生物制药科技有限公司 | Traditional Chinese medicine formulation and its novel preparation method |
| CN101422596A (en) * | 2008-11-07 | 2009-05-06 | 江西昌诺药业有限公司 | Preserved snake gall orange peel oral liquid and quality control method thereof |
| CN102552806A (en) * | 2012-01-10 | 2012-07-11 | 山东中医药大学附属医院 | Fat-burning dredging particles and preparation method thereof |
| CN103372081A (en) * | 2012-04-27 | 2013-10-30 | 江西济民可信药业有限公司 | Preparation method of Chinese herba preparation snake gall-dried orange peel oral liquid |
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