CN105999022A - Method for extracting fructus amomi volatile oil, fructus amomi flavone and fructus amomi polysaccharide by utilizing fructus amomi - Google Patents
Method for extracting fructus amomi volatile oil, fructus amomi flavone and fructus amomi polysaccharide by utilizing fructus amomi Download PDFInfo
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- CN105999022A CN105999022A CN201610350733.7A CN201610350733A CN105999022A CN 105999022 A CN105999022 A CN 105999022A CN 201610350733 A CN201610350733 A CN 201610350733A CN 105999022 A CN105999022 A CN 105999022A
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 70
- 229930003944 flavone Natural products 0.000 title claims abstract description 47
- 235000011949 flavones Nutrition 0.000 title claims abstract description 47
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 title claims abstract description 43
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 42
- 150000004676 glycans Chemical class 0.000 title claims abstract description 34
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 34
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 88
- 239000000284 extract Substances 0.000 claims abstract description 69
- 239000003814 drug Substances 0.000 claims abstract description 15
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 229940079593 drug Drugs 0.000 claims abstract description 6
- 238000001694 spray drying Methods 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 25
- 239000012567 medical material Substances 0.000 claims description 19
- 244000141331 Amomum villosum Species 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 13
- 238000012869 ethanol precipitation Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 230000009977 dual effect Effects 0.000 claims description 10
- 230000008719 thickening Effects 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000003921 oil Substances 0.000 claims description 7
- 239000004576 sand Substances 0.000 claims description 6
- KGEKLUUHTZCSIP-HOSYDEDBSA-N [(1s,4s,6r)-1,7,7-trimethyl-6-bicyclo[2.2.1]heptanyl] acetate Chemical compound C1C[C@]2(C)[C@H](OC(=O)C)C[C@H]1C2(C)C KGEKLUUHTZCSIP-HOSYDEDBSA-N 0.000 claims description 5
- 238000000703 high-speed centrifugation Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 150000002213 flavones Chemical class 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 235000013305 food Nutrition 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 238000000605 extraction Methods 0.000 description 15
- 230000001276 controlling effect Effects 0.000 description 12
- 239000000203 mixture Substances 0.000 description 6
- 239000004615 ingredient Substances 0.000 description 5
- 229930003935 flavonoid Natural products 0.000 description 4
- 150000002215 flavonoids Chemical class 0.000 description 4
- 235000017173 flavonoids Nutrition 0.000 description 4
- 239000004480 active ingredient Substances 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 235000013402 health food Nutrition 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 210000000952 spleen Anatomy 0.000 description 2
- 206010000077 Abdominal mass Diseases 0.000 description 1
- 241001127714 Amomum Species 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001605 fetal effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000346 nonvolatile oil Substances 0.000 description 1
- 230000035935 pregnancy Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- -1 sand Core flavone Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 210000000582 semen Anatomy 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/906—Zingiberaceae (Ginger family)
- A61K36/9064—Amomum, e.g. round cardamom
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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Abstract
The invention discloses a method for extracting fructus amomi volatile oil, fructus amomi flavone and fructus amomi polysaccharide by utilizing fructus amomi. The method comprises the following steps: grinding fructus amomi, heating and extracting with a volatile oil extractor; condensing vapor in the extracting process to collect the fructus amomi volatile oil; sequentially centrifuging, concentrating, performing alcohol precipitation and centrifugally separating the fructus amomi extracted raw liquor in the extrator to obtain alcohol-precipitated supernate and alcohol-precipitated precipitation; concentrating the alcohol-precipitated supernate, and performing spray drying to prepare the fructus amomi flavone extract; and drying the alcohol-precipitated precipitation by adopting a heat-circulation oven or a plate-type vacuum dryer to prepare the fructus amomi polysaccharide extract. According to the method, the fructus amomi is extracted once to obtain the fructus amomi volatile oil, fructus amomi flavone and fructus amomi polysaccharide extract simultaneously, and realizes comprehensive utilization. The prepared products can be applied to foods, medicines and other fields, so that the production cost is effectively reduced, and reasonable utilization of resources is realized. The method has remarkable economic and social benefits.
Description
Technical field
The invention belongs to the preparation method of Chinese medicine extract, be specifically related to one and utilize Fructus Amomi to extract Fructus Amomi volatile oil, sand
Core flavone and the method for Fructus Amomi polysaccharide.
Background technology
Fructus Amomi is zingiberaceous plant Fructus Amomi (Amomum villosum Lour), green shell sand (Amomum villosum
Lour. var. xanthioides T.L.Wu et Senjen) or SEMEN AMOMI LONGILIGULA (Amomum longiligularg T.L.
Wu) dry mature fruit.Fructus Amomi growth conditions is harsh, need to be grown in high temperature, moistening south subtropics, annual rainfall exist
Dark and damp, the foggy area of warm heat of more than 1000mm, such as areas such as spring in Guangdong, Gaozhou county, the shockproof of Guangxi waits area, Fructus Amomi medicine
Material per mu yield about 110 kilograms, annual Fructus Amomi yield is less.Fructus Amomi has removing dampness appetizing, warming spleen and stopping diarrha, antiabortive merit of regulating the flow of vital energy
Can, it is mainly used in turbid damp obstructing in middle-JIAO, the symptoms such as gastral cavity painful abdominal mass is the most hungry, Deficiency and coldness of spleen and stomach, and vomiting is had loose bowels, pregnancy reactions, frequent fetal movement.Fructus Amomi master
Wanting composition is volatile oil composition, but the most also contains flavones ingredient and polysaccharide composition.Therefore, extract from Fructus Amomi medical material
Fructus Amomi volatile oil or Fructus Amomi flavonoid and polysaccharide extract, as health food and the raw materials for production of medicine, become Fructus Amomi medicine
One of direction that material develops.
It is broadly divided into following two aspect currently for the exploitation of Fructus Amomi medical material:
One is to extract volatile oil composition therein, and industry is interior more to the research of this respect, has employing vapor distillation, surpasses and face
Boundary CO2The methods such as extraction, subcritical abstraction, utilize the volatile feature of volatile oil, extract volatile oil and purification, will carry
The Fructus Amomi volatile oil got is applied in various health food and medicine.But use current existing vapor distillation, supercritical
CO2After the methods such as extraction, subcritical abstraction have extracted Fructus Amomi volatile oil, the most only remain medicinal residues, do not extract
Liquid composition, is typically all the most aborning and is directly discarded by medicinal residues, causes the flavonoid in Fructus Amomi medicinal residues, polysaccharide etc. effective
Composition can not be fully utilized；Also someone want by remaining medicinal residues again with, wherein add solvent re-start extraction, return
Receive effective ingredient material therein, but this can produce again extra production cost and human cost, does not calculates.
Two is to extract fixed oil constituents therein, i.e. carries the Fructus Amomi flavone in Fructus Amomi medical material or Fructus Amomi polysaccharide
Take, few to the research of this respect in industry, it is common that to use ethanol or water directly Fructus Amomi medical material to be carried out heating extraction, will carry
Take liquid to carry out concentrating, being dried, obtain total flavonoid or total polysaccharides class extract.But during said extracted, in Fructus Amomi medical material
Volatile oil effective ingredient due to Extracting temperature high, or extraction vessel sealing is strong, direct volatilization loss, causes volatilization
Oil component is not collected and is utilized.
Therefore, the existing exploitation to Fructus Amomi medical material in industry, all it is only limitted to effective ingredient a certain in Fructus Amomi
Independent extraction and application, also do not have a kind of simultaneously by the volatile oil material in Fructus Amomi, total flavonoids substance and total polysaccharides class thing
Matter all carries out the method for comprehensive extraction and application, makes the utilization rate of Fructus Amomi medical material be substantially reduced, causes the great wasting of resources.
Summary of the invention
The purpose of the present invention is the existing exploitation to Fructus Amomi medical material in being aiming at current industry, are all only limitted to sand
The independent extraction and application of a certain effective ingredient in core, also do not have a kind of can be simultaneously by the volatile oil material in Fructus Amomi, always yellow
The method that letones and total polysaccharides class material carry out comprehensive extraction and application, the utilization rate causing Fructus Amomi medical material is low, the wasting of resources
Problem, it is provided that a kind of utilize Fructus Amomi to extract Fructus Amomi volatile oil, Fructus Amomi flavone and the method for Fructus Amomi polysaccharide.
The a kind of of the present invention utilizes Fructus Amomi to extract Fructus Amomi volatile oil, Fructus Amomi flavone and the method for Fructus Amomi polysaccharide, including following
Step:
(1) preparation of Fructus Amomi volatile oil: take Fructus Amomi medicinal raw material, adds volatile oil is drawn with disintegrating machine after broken for Fructus Amomi medical material
In device, add raw materials quality 10～the water of 15 times, soak 0.5～1.0 hour, extract 5.0～6.0 hours, steam is carried out cold
Solidifying, collect Fructus Amomi volatile oil, yield >=3.0% of Fructus Amomi volatile oil, the relative density of gained Fructus Amomi volatile oil be 0.918～
0.950, refraction index is 1.495～1.510, the content >=400mg/ml of borneol acetate；
(2) collection of amomum villosum extract: the Fructus Amomi in step (1) volatile oil extractor being extracted thick liquid and discharges, Fructus Amomi medicinal residues are abandoned
Go；Fructus Amomi extracting thick liquid disc centrifuge and carries out high speed centrifugation, arranging feeding temperature is 45～50 DEG C, charging rate
4000～5000L/h, rotating speed is 5000～6000r/min, centrifugal 40～50min, and collect centrifugal liquid and be amomum villosum extract, from
Precipitation after the heart discards；
(3) concentrating: amomum villosum extract uses dual-effect concentrator carry out concentrating under reduced pressure, controlling thickening temperature is 65～75 DEG C, dense
It is reduced to the Fructus Amomi raw material Han 1g in every 1ml concentrated solution；
(4) precipitate with ethanol: add concentrated solution volume 1.7 in concentrated solution～5.3 times of mass fractions are the edible ethanol of 95%, make concentration
In liquid, the mass fraction of ethanol reaches 60～80%, stirs, and stands 12h and obtains precipitate with ethanol solution；
(5) centrifugal: being separated by precipitate with ethanol solution employing Horizontal helical type centrifuge, rotating speed is 5000～5500r/min, respectively obtains
Precipitate with ethanol supernatant and precipitate with ethanol precipitation；
(6) preparation of Fructus Amomi flavone: precipitate with ethanol supernatant step (5) prepared uses dual-effect concentrator to carry out concentrating under reduced pressure, returns
Receiving ethanol, controlling thickening temperature is 65～80 DEG C, and vacuum is between-0.06MPa～0.09MPa, and being condensed into proportion is 1.08
～the extractum of 1.12, the extractum after concentrating is spray-dried, and controlling inlet temperature is 190～200 DEG C, and leaving air temp is 90
～100 DEG C, collect dry powder after spray drying and obtain the Fructus Amomi flavone extract powder of brown color, the yield of Fructus Amomi flavone extract
>=5.0%, total flavones >=40% in gained Fructus Amomi flavone extract, moisture≤5.0%, 80 mesh sieve percent of pass >=90%；
(7) preparation of Fructus Amomi polysaccharide: precipitate with ethanol precipitation step (5) prepared adds heat-circulation oven or board-like vacuum desiccator
In, control baking temperature and be dried at 60～80 DEG C, dried material employing Universalpulverizer is pulverized, pulverizes
Machine screen cloth >=80 mesh, obtains the Fructus Amomi polyoses extract powder of brown color, yield >=5.0% of Fructus Amomi polyoses extract, gained sand
Total polysaccharides >=15% in core polyoses extract, moisture≤5.0%, 80 mesh sieve percent of pass >=90%.
Described volatile oil extractor is that the TL200 type volatile oil produced by Hangzhou San Te medication chemistry equipment company limited carries
Take device.This volatile oil extractor is mainly made up of three parts: one is volatile oil is drawn special oil-water separator, and two is Chinese medicine
Extractor, three is automatic control cabinet.Volatile oil is drawn special oil-water separator is connected on Chinese medicament extracting device by condenser, in
Medicine extractor divides two-layer, and internal layer loads medical material and water；Interlayer is zone of heating, is passed through steam and carries out heat temperature raising in interlayer.
During extracting, when after the liquid boiling in extractor, under the effect of automatic control cabinet, it is achieved constant temperature extracts.Temperature can
To set, regulate and show, reach the purpose of A.T.C, while extracting volatile oil, during extracting solution is retained in
In medicine extractor.Certainly the volatile oil extractor in the present invention is not limited to said extracted device, as long as being capable of limit to purify volatilization
Extracting solution is produced on oil limit, and completes volatile oil and separate with extracting solution and the device of collection, all can use.
Fructus Amomi medical material, in preparation process, is first crushed by the inventive method, makes Pericarpium Amomi be broken, it is simple to follow-up
During heating extraction, Fructus Amomi volatile oil and Fructus Amomi flavone, the dissolution of Fructus Amomi polysaccharide, then carried out in special volatile oil extractor
Heating extraction, obtains Fructus Amomi and extracts while collection Fructus Amomi volatile oil by the flavone in Fructus Amomi, polysaccharide extracts active ingredients out
Thick liquid, extracts Fructus Amomi thick liquid and is centrifuged successively, concentrates, precipitate with ethanol, is centrifuged again, obtain precipitate with ethanol supernatant and precipitate with ethanol precipitation, alcohol
Heavy supernatant is spray-dried after concentrating under reduced pressure, produces Fructus Amomi flavone extract, precipitate with ethanol precipitation use heat-circulation oven or
Board-like vacuum desiccator is dried produces Fructus Amomi polyoses extract, reaches in a technical process simultaneously by Fructus Amomi volatile oil, sand
The purpose that core flavone, Fructus Amomi polysaccharide disposably extract, makes the utilization rate of Fructus Amomi medical material maximize, it is to avoid the wasting of resources, warp
The inventive method is extracted, and the yield of Fructus Amomi volatile oil reaches more than 3.0%, and the yield of Fructus Amomi flavone extract reaches more than 5.0%, Fructus Amomi
The yield of polyoses extract reaches more than 5.0%, compared with traditional individually extraction single active ingredient, and the yield difference of each product
Not quite.
The inventive method technique is simple, with low cost, once extracts by using Fructus Amomi medical material, obtains Fructus Amomi simultaneously and wave
Hair oil, Fructus Amomi flavone, Fructus Amomi polyoses extract, comprehensively utilized Fructus Amomi medical material, the product obtained can be applicable to food,
Multiple field such as medicine, effectively reduces production cost, has significant economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the technological process block-diagram of the present invention.
Detailed description of the invention
Below to utilize Fructus Amomi to extract Fructus Amomi volatile oil, Fructus Amomi flavone and sand in Jing Brand Bio-medicine Co., Ltd.'s actual production
As a example by the concrete production process of core polysaccharide, explain in detail the present invention, but they limit the present invention never in any form, specifically
The condition of production is as follows:
Embodiment 1
See Fig. 1, a kind of utilize Fructus Amomi to extract Fructus Amomi volatile oil, Fructus Amomi flavone, the method for Fructus Amomi polysaccharide, comprise the steps:
(1) preparation of Fructus Amomi volatile oil: take Fructus Amomi medicinal raw material 100kg, adds volatilization with disintegrating machine after broken for Fructus Amomi medical material
In oil extractor, add the water of 1000L, soak 0.5 hour, heating extraction 5.0 hours, steam is condensed, collects sand
Core volatile oil 3.0kg, the yield of Fructus Amomi volatile oil is 3.0%, and the relative density of gained Fructus Amomi volatile oil is 0.925, refraction index
Being 1.499, the content of borneol acetate is 454.5mg/ml；Described volatile oil extractor is by Hangzhou San Te medication chemistry equipment
The TL200 type volatile oil extractor that company limited produces；
(2) collection of amomum villosum extract: the Fructus Amomi in step (1) volatile oil extractor being extracted thick liquid and discharges, Fructus Amomi medicinal residues are abandoned
Go；Fructus Amomi extracting thick liquid disc centrifuge and carries out high speed centrifugation, arranging feeding temperature is 45 DEG C, and charging rate is
4000L/h, rotating speed is 6000r/min, centrifugal 50min, collects centrifugal liquid and is amomum villosum extract, and the precipitation after being centrifuged discards；
(3) concentrating: amomum villosum extract uses dual-effect concentrator carry out concentrating under reduced pressure, controlling thickening temperature is 65 DEG C, is concentrated into
The Fructus Amomi raw material Han 1g in every 1ml concentrated solution, obtains 100L concentrated solution；
(4) precipitate with ethanol: adding 170L mass fraction in concentrated solution is the edible ethanol of 95%, makes the quality of ethanol in concentrated solution divide
Number reaches 60%, stirs, and stands 12h and obtains precipitate with ethanol solution；
(5) centrifugal: being separated by precipitate with ethanol solution employing Horizontal helical type centrifuge, rotating speed is 5500r/min, respectively obtains on precipitate with ethanol
Clear liquid and precipitate with ethanol precipitation；
(6) preparation of Fructus Amomi flavone: precipitate with ethanol supernatant step (5) prepared uses dual-effect concentrator to carry out concentrating under reduced pressure, returns
Receiving ethanol, controlling thickening temperature is 65 DEG C, and vacuum is-0.06MPa, is condensed into the extractum that proportion is 1.08, after concentrating
Extractum is spray-dried, and controlling inlet temperature is 190 DEG C, and leaving air temp is 90 DEG C, collects dry powder and obtain palm fibre after spray drying
The Fructus Amomi flavone extract powder 7.5kg of yellow, the yield of Fructus Amomi flavone extract is 7.5%, in gained Fructus Amomi flavone extract
Total flavones is 41.7%, and moisture is 3.5%, and 80 mesh sieve percent of pass are 95%；
(7) preparation of Fructus Amomi polysaccharide: precipitate with ethanol precipitation step (5) prepared adds heat-circulation oven or board-like vacuum desiccator
In, control baking temperature and be dried at 60 DEG C, dried material employing Universalpulverizer is pulverized, crusher sifting
Net >=80 mesh, obtains the Fructus Amomi polyoses extract powder 5.0kg of brown color, and the yield of Fructus Amomi polyoses extract is 5.0%, gained
In Fructus Amomi polyoses extract, total polysaccharides is 21.5%, and moisture is 3.7%, and 80 mesh sieve percent of pass are 94%.
Embodiment 2
A kind of utilize Fructus Amomi extract Fructus Amomi volatile oil, Fructus Amomi flavone, the method for Fructus Amomi polysaccharide, comprise the steps:
(1) preparation of Fructus Amomi volatile oil: take Fructus Amomi medicinal raw material 100kg, adds volatilization with disintegrating machine after broken for Fructus Amomi medical material
In oil extractor, add the water of 1200L, soak 0.7 hour, heating extraction 5.5 hours, steam is condensed, collects sand
Core volatile oil 3.1kg, the yield of Fructus Amomi volatile oil is 3.1%, and the relative density of gained Fructus Amomi volatile oil is 0.931, refraction index
Being 1.502, the content of borneol acetate is 428.7mg/ml；Described volatile oil extractor is by Hangzhou San Te medication chemistry equipment
The TL200 type volatile oil extractor that company limited produces；
(2) collection of amomum villosum extract: the Fructus Amomi in step (1) volatile oil extractor being extracted thick liquid and discharges, Fructus Amomi medicinal residues are abandoned
Go；Fructus Amomi extracting thick liquid disc centrifuge and carries out high speed centrifugation, arranging feeding temperature is 48 DEG C, and charging rate is
4500L/h, rotating speed is 5000r/min, centrifugal 40min, collects centrifugal liquid and is amomum villosum extract, and the precipitation after being centrifuged discards；
(3) concentrating: amomum villosum extract uses dual-effect concentrator carry out concentrating under reduced pressure, controlling thickening temperature is 70 DEG C, is concentrated into
The Fructus Amomi raw material Han 1g in every 1ml concentrated solution, obtains 100L concentrated solution；
(4) precipitate with ethanol: adding 280L mass fraction in concentrated solution is the edible ethanol of 95%, makes the quality of ethanol in concentrated solution divide
Number reaches 70%, stirs, and stands 12h and obtains precipitate with ethanol solution；
(5) centrifugal: being separated by precipitate with ethanol solution employing Horizontal helical type centrifuge, rotating speed is 5300r/min, respectively obtains on precipitate with ethanol
Clear liquid and precipitate with ethanol precipitation；
(6) preparation of Fructus Amomi flavone: precipitate with ethanol supernatant step (5) prepared uses dual-effect concentrator to carry out concentrating under reduced pressure, returns
Receiving ethanol, controlling thickening temperature is 72 DEG C, and vacuum is 0.01MPa, is condensed into the extractum that proportion is 1.10, the leaching after concentrating
Cream is spray-dried, and controlling inlet temperature is 195 DEG C, and leaving air temp is 95 DEG C, collects dry powder and obtain pale brown after spray drying
The Fructus Amomi flavone extract powder 6.2kg of color, the yield of Fructus Amomi flavone extract is 6.2%, total in gained Fructus Amomi flavone extract
Flavone is 49%, and moisture is 3.1%, and 80 mesh sieve percent of pass are 97%；
(7) preparation of Fructus Amomi polysaccharide: precipitate with ethanol precipitation step (5) prepared adds heat-circulation oven or board-like vacuum desiccator
In, control baking temperature and be dried at 70 DEG C, dried material employing Universalpulverizer is pulverized, crusher sifting
Net >=80 mesh, obtains the Fructus Amomi polyoses extract powder 6.4kg of brown color, and the yield of Fructus Amomi polyoses extract is 6.4%, gained
In Fructus Amomi polyoses extract, total polysaccharides is 17.8%, and moisture is 2.9%, and 80 mesh sieve percent of pass are 93%.
Embodiment 3
A kind of utilize Fructus Amomi extract Fructus Amomi volatile oil, Fructus Amomi flavone, the method for Fructus Amomi polysaccharide, comprise the steps:
(1) preparation of Fructus Amomi volatile oil: take Fructus Amomi medicinal raw material 100kg, adds volatilization with disintegrating machine after broken for Fructus Amomi medical material
In oil extractor, add the water of 1500L, soak 1.0 hours, heating extraction 6.0 hours, steam is condensed, collects sand
Core volatile oil 3.0kg, the yield of Fructus Amomi volatile oil is 3.0%, and the relative density of gained Fructus Amomi volatile oil is 0.942, refraction index
Being 1.501, the content of borneol acetate is 445.4mg/ml；
(2) collection of amomum villosum extract: the Fructus Amomi in step (1) volatile oil extractor being extracted thick liquid and discharges, Fructus Amomi medicinal residues are abandoned
Go；Fructus Amomi extracting thick liquid disc centrifuge and carries out high speed centrifugation, arranging feeding temperature is 50 DEG C, and charging rate is
5000L/h, rotating speed is 5000r/min, centrifugal 45min, collects centrifugal liquid and is amomum villosum extract, and the precipitation after being centrifuged discards；
(3) concentrating: amomum villosum extract uses dual-effect concentrator carry out concentrating under reduced pressure, controlling thickening temperature is 75 DEG C, is concentrated into
The Fructus Amomi raw material Han 1g in every 1ml concentrated solution, obtains 100L concentrated solution；
(4) precipitate with ethanol: adding 530L mass fraction in concentrated solution is the edible ethanol of 95%, makes the quality of ethanol in concentrated solution divide
Number reaches 80%, stirs, and stands 12h and obtains precipitate with ethanol solution；
(5) centrifugal: being separated by precipitate with ethanol solution employing Horizontal helical type centrifuge, rotating speed is 5000r/min, respectively obtains on precipitate with ethanol
Clear liquid and precipitate with ethanol precipitation；
(6) preparation of Fructus Amomi flavone: precipitate with ethanol supernatant step (5) prepared uses dual-effect concentrator to carry out concentrating under reduced pressure, returns
Receiving ethanol, controlling thickening temperature is 80 DEG C, and vacuum is 0.09MPa, is condensed into the extractum that proportion is 1.12, the leaching after concentrating
Cream is spray-dried, and controlling inlet temperature is 200 DEG C, and leaving air temp is 100 DEG C, collects dry powder and obtain pale brown after spray drying
The Fructus Amomi flavone extract powder 5.1kg of color, the yield of Fructus Amomi flavone extract is 5.1%, total in gained Fructus Amomi flavone extract
Flavone is 52.6%, and moisture is 2.8%, and 80 mesh sieve percent of pass are 94%；
(7) preparation of Fructus Amomi polysaccharide: precipitate with ethanol precipitation step (5) prepared adds heat-circulation oven or board-like vacuum desiccator
In, control baking temperature and be dried at 80 DEG C, dried material employing Universalpulverizer is pulverized, crusher sifting
Net >=80 mesh, obtains the Fructus Amomi polyoses extract powder 7.4kg of brown color, and the yield of Fructus Amomi polyoses extract is 7.4%, gained
In Fructus Amomi polyoses extract, total polysaccharides is 15.6%, and moisture is 3.0%, and 80 mesh sieve percent of pass are 97%.
Claims (2)
1. one kind utilizes Fructus Amomi to extract Fructus Amomi volatile oil, Fructus Amomi flavone and the method for Fructus Amomi polysaccharide, it is characterised in that include following
Step:
(1) preparation of Fructus Amomi volatile oil: take Fructus Amomi medicinal raw material, adds volatile oil is drawn with disintegrating machine after broken for Fructus Amomi medical material
In device, add raw materials quality 10～the water of 15 times, soak 0.5～1.0 hour, extract 5.0～6.0 hours, steam is carried out cold
Solidifying, collect Fructus Amomi volatile oil, yield >=3.0% of Fructus Amomi volatile oil, the relative density of gained Fructus Amomi volatile oil be 0.918～
0.950, refraction index is 1.495～1.510, the content >=400mg/ml of borneol acetate；
(2) collection of amomum villosum extract: the Fructus Amomi in step (1) volatile oil extractor being extracted thick liquid and discharges, Fructus Amomi medicinal residues are abandoned
Go；Fructus Amomi extracting thick liquid disc centrifuge and carries out high speed centrifugation, arranging feeding temperature is 45～50 DEG C, charging rate
4000～5000L/h, rotating speed is 5000～6000r/min, centrifugal 40～50min, and collect centrifugal liquid and be amomum villosum extract, from
Precipitation after the heart discards；
(3) concentrating: amomum villosum extract uses dual-effect concentrator carry out concentrating under reduced pressure, controlling thickening temperature is 65～75 DEG C, dense
It is reduced to the Fructus Amomi raw material Han 1g in every 1ml concentrated solution；
(4) precipitate with ethanol: add concentrated solution volume 1.7 in concentrated solution～5.3 times of mass fractions are the edible ethanol of 95%, make concentration
In liquid, the mass fraction of ethanol reaches 60～80%, stirs, and stands 12h and obtains precipitate with ethanol solution；
(5) centrifugal: being separated by precipitate with ethanol solution employing Horizontal helical type centrifuge, rotating speed is 5000～5500r/min, respectively obtains
Precipitate with ethanol supernatant and precipitate with ethanol precipitation；
(6) preparation of Fructus Amomi flavone: precipitate with ethanol supernatant step (5) prepared uses dual-effect concentrator to carry out concentrating under reduced pressure, returns
Receiving ethanol, controlling thickening temperature is 65～80 DEG C, and vacuum is between-0.06MPa～0.09MPa, and being condensed into proportion is 1.08
～the extractum of 1.12, the extractum after concentrating is spray-dried, and controlling inlet temperature is 190～200 DEG C, and leaving air temp is 90
～100 DEG C, collect dry powder after spray drying and obtain the Fructus Amomi flavone extract powder of brown color, the yield of Fructus Amomi flavone extract
>=5.0%, total flavones >=40% in gained Fructus Amomi flavone extract, moisture≤5.0%, 80 mesh sieve percent of pass >=90%；
(7) preparation of Fructus Amomi polysaccharide: precipitate with ethanol precipitation step (5) prepared adds heat-circulation oven or board-like vacuum desiccator
In, control baking temperature and be dried at 60～80 DEG C, dried material employing Universalpulverizer is pulverized, pulverizes
Machine screen cloth >=80 mesh, obtains the Fructus Amomi polyoses extract powder of brown color, yield >=5.0% of Fructus Amomi polyoses extract, gained sand
Total polysaccharides >=15% in core polyoses extract, moisture≤5.0%, 80 mesh sieve percent of pass >=90%.
The most according to claim 1 a kind of Fructus Amomi is utilized to extract Fructus Amomi volatile oil, Fructus Amomi flavone and the method for Fructus Amomi polysaccharide,
It is characterized in that: described volatile oil extractor is the TL200 type volatilization produced by Hangzhou San Te medication chemistry equipment company limited
Oil extractor.
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| CN108414650A (en) * | 2018-02-09 | 2018-08-17 | 深圳市药品检验研究院（深圳市医疗器械检测中心） | Fructus amomi discrimination method and its application and system |
| CN109134695A (en) * | 2018-08-08 | 2019-01-04 | 劲牌生物医药有限公司 | A kind of alcohol-soluble beta glucan extract and preparation method thereof, application and health liquor |
| CN112961261A (en) * | 2021-03-25 | 2021-06-15 | 中山大学 | Yangchun sand rhizome polysaccharide, preparation method thereof and anti-oxidation application thereof |
| CN116349817A (en) * | 2023-04-07 | 2023-06-30 | 漳州卫生职业学院 | Fructus amomi solid beverage and preparation method thereof |
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Address after: 435000 9 Shengming Road, Jinshan street, Huangshi economic and Technological Development Zone, Hubei Province Patentee after: Jingpai Zhengtang Pharmaceutical Co.,Ltd. Address before: 435100 south of Jinshan Avenue, Jinshan Industrial Park, Huangshi City, Hubei Province Patentee before: JING BRAND BIO-MEDICINE Co.,Ltd. |