CN102416133A - Salted fructus alpiniae oxyphyllae formula particle and preparation method thereof - Google Patents
Salted fructus alpiniae oxyphyllae formula particle and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of extraction and preparation of traditional Chinese medicines, and particularly relates to a salted fructus alpiniae oxyphyllae formula particle and a preparation method thereof, aiming at providing a salted fructus alpiniae oxyphyllae formula particle with an obvious curative effect of the product and convenient administration. The preparation method comprises the following steps of: removing shells of alpinia oxyphylla medicines, adding saline solution for complete moistening, frying to be dried and obtaining salted fructus alpiniae oxyphyllae; crushing the salted fructus alpiniae oxyphyllae into rough powder, adopting supercritical carbon dioxide extraction to obtain volatile oil and medicine dregs for spare; clathrating the volatile oil with beta-cyclodextrin to obtain volatile oil-beta-cyclodextrin clathrate compound; decocting the medicine dregs with water to obtain decocted liquid, filtering, concentrating into extract, adding auxiliary materials with the amount being 15-25% of that of the extract, spraying, drying and obtaining extract powder; and adding the clathrate compound into the extract powder, carrying out dry-process granulation and obtaining the particle. The invention has the advantages that the strict standard is formulated in the aspects of shell removing process, the salting process, the quality of the raw medicine pieces and the like, and in the aspect of the pharmacological and pharmacodynamic test, the obvious effect of urine reduction of the product is ensured; and simultaneously the cost is low, the storage is easy, the carrying and the administration are convenient and the like.
Description
Technical field
The invention belongs to Chinese medicine extraction and formulation art, be specifically related to stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule and preparation method thereof.
Background technology
Fructus Alpiniae Oxyphyllae is the zingiberaceous plant Fructus Alpiniae Oxyphyllae
Alpinia oxyphyllaMiq. dry mature fruit is a tcm clinical practice Chinese medicine simply commonly used.Fructus Alpiniae Oxyphyllae is given birth to the hot temperature of article and dry, and the master returns spleen channel, takes the photograph saliva and spittle power with warming spleen and stopping diarrha, receipts and wins, diseases such as the stomachache that is usually used in Deficiency and coldness of spleen and stomach is vomited and diarrhoea, mouthful saliva gravity flow; After processing, salt can relax hot dry property, the main kidney channel of returning, and the specially capable part of the body cavity below the umbilicus, housing the bladder, kidneys and bowels is longer than controlling nocturnal emission with astringent drugs, reducing urination, and diseases such as many seminal emissions in order to treatment kidney qi deficiency and coldness, premature ejaculation, frequent micturition, the enuresis, nebulousurine are to be used as medicine to strengthen the effect of the kidney warming reducing urination with stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution like Pill for Decreasing Urination.
In recent years, along with the variation of human diseases spectrum, the toxic and side effects of some chemicalses is gradually by people's understanding, and Chinese medicine more and more receives the people of other countries' favor with the uniqueness of its curative effect and the naturality in its source.And the application method of Chinese medicine " decoction pieces is used as medicine; face with frying in shallow oil soup "; Incompatibility modern's rhythm of life; The uncontrollability of its product quality, the uncertainty of clinical efficacy more and more do not conform to development of modern scientific technology, and therefore, integrated modern science and technology method is arisen at the historic moment with advanced Chinese medicine preparation technology, the Chinese medicinal granule of detection means.It is to be raw material with the prepared slices of Chinese crude drugs that meet concocted specification, through modern industry extract, concentrate, dry, the refining pure Chinese medicine series of products that form of granulating, its nature and flavor, return through, effect consistent with the former prepared slices of Chinese crude drugs.Replace the prepared slices of Chinese crude drugs to supply the clinical syndrome differentiation opinion to control, add and subtract with it with card; Prescription uses; The property of medicine drug effect that had both kept the former prepared slices of Chinese crude drugs; Do not have the adjustment of need decocting, be easy to, convenient use, quality controllable fast again, more meet modern's consumption and life requirement, be prone to also accept for domestic and international consumer acceptance.
At present, existing stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule production marketing on the market, but also there is following problem in this product at aspects such as production and quality controls:
1. traditional Fructus Alpiniae Oxyphyllae medical material technology of shelling is loaded down with trivial details, wastes time and energy
Traditional Fructus Alpiniae Oxyphyllae method of shelling adopts manual crushing to shell more, or mill groove pulverizes and shell, or earlier Fructus Alpiniae Oxyphyllae is fried to cokled surface, uses the flattening mill grating then, and selecting crude drugs with winnower is removed decapsidate subsequently, and this method is time-consuming, and the Fructus Alpiniae Oxyphyllae yield is not high, is not suitable for big production.
2. can't guarantee stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule quality from the source
Chinese medicinal granule is to be raw material with the prepared slices of Chinese crude drugs that meet concocted specification, and therefore, the quality of prepared slice quality directly influences the granule quality.At present, stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution processing procedure and quality control still can't be calibrated and will definitely comply with.Version Chinese Pharmacopoeia in 2010 is processed technology for " getting Fructus Alpiniae Oxyphyllae; fry by the saline method of processing and do " about Fructus Alpiniae Oxyphyllae salt, does not have concrete technological parameter, and quality of medicinal material control still only with volatile oil content as standard; Be difficult to guarantee and control stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution prepared slice quality, can't guarantee the granule quality from the source.
3. stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution volatile oil extraction ratio is not high
The stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution traditional extraction technique normally adopts steam distillation to extract volatile oil, and medicinal residues exist the volatile oil extraction ratio not high with all the other compositions of water boiling and extraction, and is prone to the adhesion wall and loses, thereby influences product quality and clinical efficacy.
Based on the industry present situation; The stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule of the present invention's preparation has both solved the granule raw material production from the decoction pieces aspect wastes time and energy and quality problems; Again from having solved the incomplete difficult problem of traditional extraction technique; And remove former decoction pieces inanimate object active component, reduced dose, easy to carry and transport.
Summary of the invention
The object of the invention is to provide a kind of stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule method for preparing, and this method crude drug source is reliable, and extraction efficiency is high, the technology simple possible.
The present invention realizes through following technical scheme, a kind of method for preparing the stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule, and this method feature is to comprise following process: adopt the rice skinning machine to slough shell the Fructus Alpiniae Oxyphyllae medical material, and the process of preparing Chinese medicine obtains the stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces.Stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution is ground into coarse powder, adopts supercritical carbon dioxide extraction method to extract volatile oil, gained volatile oil is used beta-cyclodextrin inclusion compound, processes volatile oil-Benexate Hydrochloride, and wherein volatile oil is 1:2～8 with the ratio of The quality of ss-cyclodextrin; The medicinal residues water decocts 3 times, adds 6～12 times of water gagings at every turn, decocts 1～2h, and merging filtrate is condensed into extractum, adds the beta-schardinger dextrin-of extractum consumption 15～25%, and spray drying is processed extract powder; Last extract powder adds clathrate, and dry granulation gets the stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule.
The invention has the advantages that preparation process is simple, parameter is prone to control.At first the technology of shelling, the salt of stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces are processed technology and prepared slice quality control aspect is studied and promoted from the granule source, obtain technological specification, quality controllable stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces; Adopt supercritical carbon dioxide extraction method, beta-cyclodextrin inclusion compound technology to prepare the stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule then, not only solved problems such as not high, the easy adhesion wall of Fructus Alpiniae Oxyphyllae volatile oil extraction efficiency, but also strengthened the dissolubility of product; Also proved that through the comparative efficacy test stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule reducing urination action effect of the present invention is remarkable at last.
Description of drawings
Fig. 1 stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution petroleum ether part GC/MS ion figure;
Fig. 2 stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces thin-layer chromatogram (1. grapefruit ketone reference substance 2. control medicinal materials 3～12. stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces);
Fig. 3 grapefruit ketone UV scanning figure;
Fig. 4 stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces HPLC collection of illustrative plates (A grapefruit ketone solution B stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution sample solution).
Specific embodiments
Below explain, but do not limit the present invention through the description of specific embodiments of the invention.
One, stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces and the comparative study of granule drug effect
Select 90 of the qualified male mices of Aston method screening for use, be divided into 6 groups at random by urine amount, body weight: model group, Pill for Decreasing Urination group, decoction pieces high and low dose group, granule high and low dose group, 15 every group.Each administration group gives corresponding medicinal liquid by the 0.4ml/20g body weight, and model group gives the equal-volume pure water, successive administration 7 days.Wherein the 6th day evening water is can't help in the animal fasting and spend the night, after the administration in the 7th day (or feedwater), each treated animal is loaded as water by 0.6ml/20g body weight filling stomach pure water behind the 1h; Squeeze the surplus urine of bladder to the greatest extent; Put in the mice metabolic cage, measure urine amount hourly in the 6h, calculate urine weight/body weight.The result sees table 1.
Table 1 stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces and granule are to the influence of water load frequent micturition model mice urine amount
| Group | Urine weight/body weight (g/g) |
| Model group | 0.0355±0.0111 |
| The Pill for Decreasing Urination group | 0.0210±0.0068 ** |
| The decoction pieces low dose group | 0.0312±0.0089 |
| The decoction pieces high dose group | 0.0235±0.0091 * |
| The granule low dose group | 0.0297±0.0093 |
| The granule high dose group | 0.0213±0.0057 ** |
Annotate: administration group and model group compare, * P 0.05, * * P < 0.01.
Compare with model group; Stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces and granule low dose group all have reducing urination trend; But no difference of science of statistics, the decoction pieces high dose group is compared with model group, has significant difference (P < 0.05); The granule high dose group is then had a utmost point significant difference (P < 0.01), show decoction pieces be prepared into granule after drug action strengthen.
Two, stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution prepared slice quality Control Study
Discover that Fructus Alpiniae Oxyphyllae Petroleum ether extraction position and Sal are brought into play the effect of the kidney warming reducing urination jointly, through petroleum ether part is analyzed discovery, grapefruit ketone accounts for more than 25% of the total composition of petroleum ether part.Therefore, select grapefruit ketone and sodium chloride as stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution prepared slice quality controlling index.Petroleum ether part GC/MS collection of illustrative plates is seen Fig. 1.
Ground such as sample picks up from the fine jade of Hainan respectively, Qionghai, Haikou, Wanning, Sanya, Guangdong, Guangxi.
The mensuration of moisture, ash, ethanol-soluble extractives, volatile oil
With reference to " method of Chinese pharmacopoeia version in 2010, the mensuration result of 10 lot sample article sees table 2.
Thin layer is differentiated
Get stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution coarse powder 2 g, add 95% ethanol of 30 mL cable-styled be extracted into colourless, the filtrating evaporate to dryness, residue is with 10 mL dissolve with methanol, as need testing solution.Other gets Fructus Alpiniae Oxyphyllae control medicinal material 2 g, shines medical material solution in pairs with legal system.Get grapefruit ketone reference substance again, add methanol and process the solution that per 1 mL contains 1 mg, as reference substance solution.According to thin layer chromatography (appendix VI B) test, draw each 10 μ L of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with petroleum ether (60～90 ℃)-ethyl acetate (9:1); Launch, take out, dry; Spray the colour developing of 5% vanillin-concentrated sulphuric acid, 105 ℃ to be heated to spot colors obvious, puts under the uviol lamp (365 nm) and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph, show same color fluorescence speckle.See Fig. 2.
2.3 assay
2.3.1 grapefruit ketone content
2.3.1.1 the chromatographic condition chromatographic column is Diamonsil-C
18Post (5 μ m, 250mm * 4.6mm); Mobile phase is acetonitrile-water (65 ︰ 35); Detecting wavelength is 235 nm; Flow velocity is 1.0mLmin
-1Column temperature is 35 ℃.Under selected condition, other component chromatographic peaks reach baseline separation in grapefruit ketone and the sample, and its theoretical cam curve (N) is greater than 4000.See Fig. 3,4:
2.3.1.2 it is an amount of that the preparation precision of reference substance solution takes by weighing grapefruit ketone reference substance, processes every 1mL with the methanol dilution and contain grapefruit ketone 0.4800 mg reference substance stock solution.Get a certain amount of reference substance stock solution, using the methanol dilution is 0.0192 mg
ML
-1 Reference substance solution.
2.3.1.3 about 0.2 g of stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution coarse powder is got in the preparation of need testing solution, the accurate title, decide, and puts in the tool plug conical flask, adds methanol 25 mL; Claim to decide weight, supersound extraction 30 min are put and are chilled to room temperature, claim to decide weight again; Supply with methanol and to subtract weight loss, shake up, filter; Get subsequent filtrate, filter, promptly get with microporous filter membrane (0.45 μ m).
2.3.1.4 linear relationship is investigated precision and is got grapefruit ketone reference substance solution sample introduction 6,8,10,12,14 μ L mensuration peak area respectively.With the reference substance sample size is abscissa, and peak area value is a vertical coordinate drawing standard curve, gets regression equation to be: A=3237.2C+4.33, r=0.9999.Show that grapefruit ketone is good linear relationship with peak area in 0.1152～0.2688 μ g scope.
2.3.1.5 the above-mentioned reference substance solution 10 μ L of the accurate absorption of precision test repeat sample introduction 5 times, peak area RSD=0.20% shows that the precision of instrument is good.
2.3.1.6 replica test is got 5 parts of same lot sample article, presses the method for preparing preparation of need testing solution respectively, sample introduction 10 μ L measure peak area, calculate content.Its RSD=1.23% shows that this method repeatability is good.
2.3.1.7 stability test is got same need testing solution, respectively at 0,2,4,6,8 hour sample introduction 10 μ l, measures peak area, calculates content.Its RSD=0.32% shows that need testing solution is stable in 8 hours.
2.3.1.8 the sample of 6 parts of known content is got in the average recovery test, content is 2.10mgg
-1About 0.1 g, the accurate title, decide, and adds grapefruit ketone reference substance solution (0.4800 mgmL respectively
-1) 0.5ml.Press the method for preparing preparation of need testing solution, sample introduction 10 μ L measure peak area, calculate recovery rate.Average recovery rate is 97.34% as a result, RSD=1.48%.It is better to show that this method is measured grapefruit ketone content accuracy.
2.3.1.9 sample size is measured: get the different batches sample powder, be equipped with need testing solution by 2.3.1.3 item below legal system, sample introduction 10 μ L measure by chromatographic condition under the 2.3.1.1 item, and the record chromatographic peak area calculates content, and the result sees table 2.
The adjuvant assay
2.3.2.1 electrode pretreatment
It is preceding in 10 that chloride ion selects electrode to use
-3MoL
-1Soak activation 1h in the KCl solution, clean repeatedly to the baseline potential value with redistilled water and reach about 270mV, can use.
2.3.2.2 instrument uses and to get solution to be measured, puts 50 mL and does in the clean beaker of behaviour, inserts chloride electrode and the 217 type calomel electrodes handled, under electromagnetic agitation, treat potential balance after (variation is no more than l mV), write down corresponding potential value (E).
2.3.2.3 the preparation of standard solution
Sodium chloride standard reagent 2.92647 g that precision takes by weighing 600 ℃ of calcination to constant weights in resistance furnace put in the 50 mL measuring bottles, use 0.10 molL
-1KNO
3The solution dissolving also is diluted to scale, shakes up, and promptly gets the NaCl solution of 1mol/L; Precision is measured 10 mL, puts in the 100 mL measuring bottles, uses 0.10 molL
-1KNO
3The solution dissolving also is diluted to scale, shakes up, and promptly gets 0.1 molL
-1NaCl solution; Get 10 with this stepwise dilution
-2～10
-4MolL
-1NaCl solution, to be measured.
2.3.2.4 stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution powder (cross No. two sieve) 1.0 g are got in the preparation of need testing solution, accurately claim surely, put in the 50mL triangular flask, add water 40 mL, supersound process 10 min are put coldly, filter, and add 1.0 molL
-1KNO
35 mL, water is settled to scale and promptly gets.
2.3.2.5 linear relationship is investigated and is got above-mentioned 10
0～10
-4MolL
-1Standard solution, the method for pressing under the 2.3.2.2 item is measured potential value, (logC) be abscissa, potential value (E) is a vertical coordinate drawing standard curve, must regression equation be Y=52.8X+0.6, and correlation coefficient is 0.9994 with the negative logarithm of concentration of standard solution.Show that chlorine ion concentration is 10
0～10
-4MolL
-1Scope in, linear relationship is good, lowest detection is limited to 1 * 10
-4MolL
-1
2.3.2.6 need testing solution is got in the precision test, replication 5 times, and the record potential value, potential value RSD=0.34% shows that instrument precision is good.
2.3.2.7 stability test is got same need testing solution, measures calculating content respectively at 0,1,2,4,6 hour.Its RSD=0.41% shows that need testing solution is stable in 6 hours.
2.3.2.8 replica test
Get 5 parts of same lot sample article, the accurate title, decide, and presses a need testing solution preparation preparation down respectively, and the mensuration potential value calculates content, and its RSD=3.29% shows that repeatability is good.
2.3.2.9 each 0.5g of sample of 6 parts of known content is got in the average recovery test, the accurate respectively sodium chloride standard reagent that adds adds the about 40mL of redistilled water more respectively, presses preparation need testing solution under the need testing solution item, measures potential value, calculate recovery rate.Average recovery rate is 98.03% as a result, RSD=2.55%, and it is good to show that application of sample reclaims.
2.3.2.10 assay method is got the different batches sample powder, is equipped with need testing solution by 2.3.2.4 item below legal system, measures by condition under the 2.3.2.2 item, the record potential value calculates content, and the result sees table 2.
Moisture, ash, ethanol-soluble extractives, volatile oil, grapefruit ketone and sodium chloride content are measured result (n=2) in the table 2 stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces
10 batches of each index meansigma methodss of stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces are: moisture 9.49%, total ash 6.33%, acid-insoluble ash 0.73%, ethanol-soluble extractives 19.10%, volatile oil 1.28%, grapefruit ketone 0.19%, sodium chloride 2.41%.According to experimental result and take all factors into consideration various influence factors; Stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution prepared slice quality standard is tentative to be: moisture must not cross 12%, and total ash must not cross 10%, and acid-insoluble ash must not cross 1.0%; Ethanol-soluble extractives must not be less than 15%; Volatile oil must not be less than 1.0%, and grapefruit ketone must not be less than 0.15%, and sodium chloride must not be less than 1.50%.
Three, preparation instance
Get stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces 100kg, be ground into coarse powder, use supercritical carbon dioxide extraction, extracting pressure is 15Mpa, and extraction temperature is 40 ℃, gets volatile oil 3kg; The beta-cyclodextrin inclusion compound legal system is equipped with Fructus Alpiniae Oxyphyllae volatile oil-Benexate Hydrochloride 21kg, and is subsequent use.Coarse powder after the extraction is dropped in the extraction pot, add the water steaming and decocting 2 times, one fries in shallow oil and adds 10 times of water gagings, decocts 240min; Two fry in shallow oil and add 8 times of water gagings, decoct 60min, merge decoction liquor twice, filter; Filtrating is evaporated to relative density under vacuum 0.1Mpa be 1.13 extractum (80 ℃); Add beta-schardinger dextrin-18kg and mixing; Spray drying, 195 ℃ of inlet temperatures, 95 ℃ of outlet temperatures are processed extract powder 20kg; Add Fructus Alpiniae Oxyphyllae volatile oil-Benexate Hydrochloride; Dry granulation gets stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule 41kg, after packing, gets product.
Get stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces 100kg, be ground into coarse powder, use supercritical carbon dioxide extraction, extracting pressure is 17Mpa, and extraction temperature is 38 ℃, gets volatile oil 2.7kg; The beta-cyclodextrin inclusion compound legal system is equipped with Fructus Alpiniae Oxyphyllae volatile oil-Benexate Hydrochloride 18.9kg, and is subsequent use.Coarse powder after the extraction is dropped in the extraction pot, add the water steaming and decocting 2 times, one fries in shallow oil and adds 10 times of water gagings, decocts 200min; Two fry in shallow oil and add 8 times of water gagings, decoct 60min, merge decoction liquor twice, filter; Filtrating is evaporated to relative density under vacuum 0.1Mpa be 1.13 extractum (80 ℃); Add beta-schardinger dextrin-16.2kg and mixing; Spray drying, 195 ℃ of inlet temperatures, 94 ℃ of outlet temperatures are processed extract powder 19kg; Add Fructus Alpiniae Oxyphyllae volatile oil-Benexate Hydrochloride; Dry granulation gets stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule 37.9kg, after packing, gets product.
Instance 3
Get stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution decoction pieces 100kg, be ground into coarse powder, use supercritical carbon dioxide extraction, extracting pressure is 16Mpa, and extraction temperature is 37 ℃, gets volatile oil 3.2kg; The beta-cyclodextrin inclusion compound legal system is equipped with Fructus Alpiniae Oxyphyllae volatile oil-Benexate Hydrochloride 22.4kg, and is subsequent use.Coarse powder after the extraction is dropped in the extraction pot, add the water steaming and decocting 2 times, one fries in shallow oil and adds 10 times of water gagings, decocts 220min; Two fry in shallow oil and add 8 times of water gagings, decoct 60min, merge decoction liquor twice, filter; Filtrating is evaporated to relative density under vacuum 0.1Mpa be 1.13 extractum (80 ℃); Add beta-schardinger dextrin-19.2kg and mixing; Spray drying, 190 ℃ of inlet temperatures, 93 ℃ of outlet temperatures are processed extract powder 19.5kg; Add Fructus Alpiniae Oxyphyllae volatile oil-Benexate Hydrochloride; Dry granulation gets stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule 41.9kg, after packing, gets product.
Claims (7)
1. the method for preparing of stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution granule is characterized in that, it adopts the following steps preparation:
A, Fructus Alpiniae Oxyphyllae medical material are removed shell and are got Fructus Alpiniae Oxyphyllae (technology of shelling);
B, Fructus Alpiniae Oxyphyllae add 10% saline solution, mix thoroughly, and moistening 30 minutes is put the interior parch of preheating medicine roasting machine 56～65 minutes, takes the dish out of the pot, and airing promptly gets stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution;
C, stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution is ground into coarse powder;
D, stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution coarse powder adopt supercritical carbon dioxide extraction to get volatile oil, and medicinal residues are subsequent use, and extracting pressure is 5～20MPa, and extraction temperature is 10～40 ℃;
E, gained volatile oil are used beta-cyclodextrin inclusion compound, get volatile oil-Benexate Hydrochloride;
F, with step D gained medicinal residues water decoct decoction liquor;
G, decoction liquor are filtered, and are condensed into extractum, add the beta-schardinger dextrin-of extractum consumption 15～25%, and drying is processed extract powder;
H, extract powder add volatile oil-Benexate Hydrochloride, and dry granulation gets final product.
2. the method for preparing of Fructus Alpiniae Oxyphyllae granule according to claim 1 is characterized in that: the steps A Fructus Alpiniae Oxyphyllae technology of shelling does, adopts the Oryza sativa L. skinning machine to remove Fructus Alpiniae Oxyphyllae medical material shell, and every 100kg Fructus Alpiniae Oxyphyllae medical material makes Fructus Alpiniae Oxyphyllae 60～75kg.
3. the method for preparing of Fructus Alpiniae Oxyphyllae granule according to claim 1; It is characterized in that: step belit Fructus Alpiniae Oxyphyllae adopts the CZY700 medicine roasting machine to make; This medicine roasting machine is by there being non-infrared contact thermography probe, can guarantee that salt is processed to monitor the medical material surface temperature in the process at any time; Fry the medicine temperature and be controlled at 115-127 ℃, the yield of stir-baked FRUCTUS ALPINIAE OXY-PHYLLAE after sprinking salt solution is 91.0%-94.0%, and every 100kg Fructus Alpiniae Oxyphyllae is used 2kg Sal.
4. the method for preparing of Fructus Alpiniae Oxyphyllae granule according to claim 1 is characterized in that: adopt an extractor, two separators during step D supercritical extraction.
5. the method for preparing of Fructus Alpiniae Oxyphyllae granule according to claim 1; It is characterized in that: step e volatile oil adopts beta-cyclodextrin inclusion compound; Wherein volatile oil is 1:2～8 with the ratio of The quality of ss-cyclodextrin, and the enclose temperature is 35～65 ℃, and the enclose time is 1～2h.
6. the method for preparing of Fructus Alpiniae Oxyphyllae granule according to claim 1 is characterized in that: step F Chinese medicine slag decocting condition is decocte with water 3 times, and each 6～12 times of water gagings decoct 1～2h.
7. the method for preparing of Fructus Alpiniae Oxyphyllae granule according to claim 1 is characterized in that: the said drying of step G is a spray drying.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103800784A (en) * | 2014-02-12 | 2014-05-21 | 谢毅强 | Fructus alpiniae oxyphyllae and compatible lindera aggregata extract for treating diabetes, and preparation method thereof |
| CN111870619A (en) * | 2020-09-09 | 2020-11-03 | 广东一方制药有限公司 | Radix angelicae pubescentis traditional Chinese medicine formula granules and preparation method thereof |
| CN113416608A (en) * | 2021-06-29 | 2021-09-21 | 中国热带农业科学院热带作物品种资源研究所 | Extraction method of intelligence-developing essential oil for inhibiting listeria monocytogenes and intelligence-developing essential oil |
| CN116392557A (en) * | 2023-04-28 | 2023-07-07 | 江西绿天食品有限公司 | Fructus alpiniae oxyphyllae extract and extraction process thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101933962A (en) * | 2010-09-13 | 2011-01-05 | 四川新绿色药业科技发展股份有限公司 | Ligusticum wallichii formulation granule and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101933962A (en) * | 2010-09-13 | 2011-01-05 | 四川新绿色药业科技发展股份有限公司 | Ligusticum wallichii formulation granule and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103800784A (en) * | 2014-02-12 | 2014-05-21 | 谢毅强 | Fructus alpiniae oxyphyllae and compatible lindera aggregata extract for treating diabetes, and preparation method thereof |
| CN111870619A (en) * | 2020-09-09 | 2020-11-03 | 广东一方制药有限公司 | Radix angelicae pubescentis traditional Chinese medicine formula granules and preparation method thereof |
| CN113416608A (en) * | 2021-06-29 | 2021-09-21 | 中国热带农业科学院热带作物品种资源研究所 | Extraction method of intelligence-developing essential oil for inhibiting listeria monocytogenes and intelligence-developing essential oil |
| CN116392557A (en) * | 2023-04-28 | 2023-07-07 | 江西绿天食品有限公司 | Fructus alpiniae oxyphyllae extract and extraction process thereof |
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Application publication date: 20120418 |