CN105999022B - A method of amomum fruit volatile oil, fructus amomi flavones and fructus amomi polysaccharide are extracted using fructus amomi - Google Patents
A method of amomum fruit volatile oil, fructus amomi flavones and fructus amomi polysaccharide are extracted using fructus amomi Download PDFInfo
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 73
- 241001127714 Amomum Species 0.000 title claims abstract description 44
- 235000013399 edible fruits Nutrition 0.000 title claims abstract description 42
- 229930003944 flavone Natural products 0.000 title claims abstract description 29
- 235000011949 flavones Nutrition 0.000 title claims abstract description 29
- 150000002213 flavones Chemical class 0.000 title claims abstract description 24
- 150000004676 glycans Chemical class 0.000 title claims abstract description 24
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 24
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000000284 extract Substances 0.000 claims abstract description 71
- 238000001556 precipitation Methods 0.000 claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 31
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N flavone Chemical compound O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003814 drug Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 230000001376 precipitating effect Effects 0.000 claims abstract description 14
- 239000006228 supernatant Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 229940079593 drug Drugs 0.000 claims abstract description 8
- 235000019441 ethanol Nutrition 0.000 claims description 51
- 244000141331 Amomum villosum Species 0.000 claims description 17
- 239000012141 concentrate Substances 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 11
- 230000009977 dual effect Effects 0.000 claims description 10
- 230000008719 thickening Effects 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229920002472 Starch Polymers 0.000 claims description 8
- 235000019698 starch Nutrition 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 5
- 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 claims description 5
- 150000002212 flavone derivatives Chemical class 0.000 claims description 5
- 230000005484 gravity Effects 0.000 claims description 5
- 238000000703 high-speed centrifugation Methods 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 5
- 238000001694 spray drying Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 19
- 238000010438 heat treatment Methods 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000000047 product Substances 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract description 2
- 235000013305 food Nutrition 0.000 abstract description 2
- 229930003935 flavonoid Natural products 0.000 description 7
- 150000002215 flavonoids Chemical class 0.000 description 7
- 235000017173 flavonoids Nutrition 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 235000013402 health food Nutrition 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 210000000952 spleen Anatomy 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- 206010000234 Abortion spontaneous Diseases 0.000 description 1
- 206010000242 Abortion threatened Diseases 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 208000005420 Hyperemesis Gravidarum Diseases 0.000 description 1
- 208000005985 Threatened Abortion Diseases 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 208000015994 miscarriage Diseases 0.000 description 1
- 239000000346 nonvolatile oil Substances 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
- 210000000582 semen Anatomy 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 208000000995 spontaneous abortion Diseases 0.000 description 1
- 210000002784 stomach Anatomy 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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- 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
Amomum fruit volatile oil is extracted using fructus amomi the invention discloses a kind of, the method of fructus amomi flavones and fructus amomi polysaccharide, it is to carry out heating extraction with volatile oil extractor after being crushed fructus amomi medicinal material, condensation collection is carried out to the steam of extraction process first and obtains amomum fruit volatile oil, then crude liquid is extracted to the fructus amomi in extractor to be successively centrifuged, concentration, alcohol precipitation, it is centrifugated again, obtain alcohol precipitation supernatant and alcohol precipitation precipitating, alcohol precipitation supernatant is spray-dried after being concentrated under reduced pressure, produce fructus amomi chromocor extract, alcohol precipitation precipitating produces fructus amomi polyoses extract using heat-circulation oven or the drying of board-like vacuum desiccator；The method of the present invention is by once extracting fructus amomi medicinal material, amomum fruit volatile oil, fructus amomi flavones, fructus amomi polyoses extract are obtained simultaneously, fructus amomi medicinal material is comprehensively utilized, obtained product can be applied to the multiple fields such as food, drug, effectively reduce production cost, the reasonable utilization of resource is realized, there is significant economic benefit and social benefit.
Description
Technical field
The invention belongs to the preparation methods of Chinese medical extract, and in particular to a kind of to extract amomum fruit volatile oil, sand using fructus amomi
The method of benevolence flavones and fructus amomi polysaccharide.
Background technique
Fructus amomi is zingiberaceous plant amomum viosum (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, wet south subtropics, annual rainfall and exist
The foggy area of the dark and damp of 1000mm or more, warm heat, such as spring, Gaozhou county area in Guangdong, the shockproof equal areas in Guangxi, fructus amomi medicine
110 kilograms of material per mu yield or so, annual fructus amomi yield is less.Fructus amomi has dampness elimination appetizing, warming spleen and stopping diarrha, regulating the flow of vital energy and preventing miscarriage function
Can, it is mainly used for turbi damp obstructing in middle-JIAO, gastral cavity ruffian is not hungry, deficiency-cold in spleen and stomach, vomiting and diarrhea, hyperemesis gravidarum, the symptoms such as threatened abortion.Fructus amomi master
Wanting ingredient is volatile oil component, but wherein also contains flavones ingredient and polysaccharide component.Therefore, it is extracted from fructus amomi medicinal material
Amomum fruit volatile oil or fructus amomi flavonoids and polysaccharide extract become fructus amomi medicine as the raw materials for production of health food and drug
One of the direction of material development and utilization.
In terms of being broadly divided into following two for the development and utilization of fructus amomi medicinal material at present:
It is more to the research of this respect in industry first is that extract volatile oil component therein, have using steam distillation,
Supercritical CO2The methods of extraction, subcritical abstraction, using the volatile feature of volatile oil, extract volatile oil and purify,
The amomum fruit volatile oil extracted is applied in various health foods and drug.But using current existing steam distillation, surpass
Critical CO2After extraction, the methods of subcritical abstraction have extracted amomum fruit volatile oil, the substantially only residue dregs of a decoction, do not have in a reservoir
Extracting solution ingredient is typically all directly to discard the dregs of a decoction, leads to flavonoids, the polysaccharide etc. in the fructus amomi dregs of a decoction in production at present
Effective component cannot be fully utilized；Also someone wants again to utilize the remaining dregs of a decoction, and addition solvent, which re-starts, wherein mentions
It takes, recycles effective component substance therein, but this can generate additional production cost and human cost again, economically very not
It is cost-effective.
Second is that extract fixed oil constituents therein, i.e., in fructus amomi medicinal material fructus amomi flavones or fructus amomi polysaccharide mention
It takes, it is few to the research of this respect in industry, heating extraction is directly usually carried out to fructus amomi medicinal material using ethyl alcohol or water, will be mentioned
It takes liquid to be concentrated, dried, obtains total flavonoid or total starches class extract.But during said extracted, in fructus amomi medicinal material
Volatile oil effective component since Extracting temperature is high or extraction vessel leakproofness is not strong, direct volatilization loss causes to volatilize
Oil component is not collected and is utilized.
Therefore, the existing development and utilization to fructus amomi medicinal material in industry are all only limitted to effective component a certain in fructus amomi
Independent extraction and application, there are no a kind of simultaneously by volatile oil substance, total flavonoids substance and the total starches class object in fructus amomi
The method that matter all carries out comprehensive extraction and application, substantially reduces the utilization rate of fructus amomi medicinal material, causes the great wasting of resources.
Summary of the invention
The purpose of the present invention is to the development and utilization to fructus amomi medicinal material existing in current industry, are all only limitted to sand
The independent extraction and application of a certain effective component in benevolence, there are no it is a kind of can be simultaneously by the volatile oil substance, total yellow in fructus amomi
The method that letones and total starches substance carry out comprehensive extraction and application, causes that the utilization rate of fructus amomi medicinal material is low, the wasting of resources
The problem of, a kind of method for extracting amomum fruit volatile oil, fructus amomi flavones and fructus amomi polysaccharide using fructus amomi is provided.
A kind of method for extracting amomum fruit volatile oil, fructus amomi flavones and fructus amomi polysaccharide using fructus amomi of the invention, including it is following
Step:
(1) preparation of amomum fruit volatile oil: taking fructus amomi medicinal raw material, and volatile oil is added after being crushed fructus amomi medicinal material with crusher
In extractor, 10~15 times of material quality of water is added, impregnates 0.5~1.0 hour, extracts 5.0~6.0 hours, to steam into
Row condensation, collects amomum fruit volatile oil, yield >=3.0% of amomum fruit volatile oil, and the relative density of gained amomum fruit volatile oil is 0.918
~0.950, refraction index is 1.495~1.510, content >=400mg/ml of Bronyl acetate；
(2) fructus amomi in step (1) volatile oil extractor the collection of amomum villosum extract: is extracted into crude liquid discharge, fructus amomi medicine
Slag discards；Fructus amomi is extracted into crude liquid and carries out high speed centrifugation with disc centrifuge, setting feeding temperature is 45~50 DEG C, charging speed
4000~5000L/h is spent, revolving speed is 5000~6000r/min, is centrifuged 40~50min, and collecting centrifugate is amomum villosum extract,
Precipitating after centrifugation discards；
(3) it is concentrated: amomum villosum extract being concentrated under reduced pressure using dual-effect concentrator, control thickening temperature is 65~75
DEG C, it is concentrated into the raw material of fructus amomi containing 1g in every 1ml concentrate；
(4) alcohol precipitation: the edible alcohol that 1.7~5.3 times of mass fractions of the volume of the concentrated liquid are 95% is added in concentrate, makes
The mass fraction of ethyl alcohol reaches 60~80% in concentrate, stirs evenly, and stands 12h and obtains alcohol precipitation solution；
(5) it is centrifuged: alcohol precipitation solution being separated using Horizontal helical type centrifuge, revolving speed is 5000~5500r/min, respectively
Obtain alcohol precipitation supernatant and alcohol precipitation precipitating；
(6) preparation of fructus amomi flavones: by alcohol precipitation supernatant made from step (5) using dual-effect concentrator depressurize it is dense
Ethyl alcohol is recycled in contracting, and control thickening temperature is 65~80 DEG C, and between -0.06MPa~0.09MPa, be condensed into specific gravity is vacuum degree
Medicinal extract after concentration is spray-dried by 1.08~1.12 medicinal extract, and control inlet air temperature is 190~200 DEG C, leaving air temp
It is 90~100 DEG C, dry powder is collected after spray drying and obtains the fructus amomi chromocor extract powder of brown color, fructus amomi chromocor extract
Yield >=5.0%, general flavone >=40% in gained fructus amomi chromocor extract, moisture≤5.0%, 80 mesh percent of pass >=90%；
(7) preparation of fructus amomi polysaccharide: alcohol precipitation made from step (5) is precipitated, heat-circulation oven or board-like vacuum drying is added
In device, control drying temperature is dried at 60~80 DEG C, the material after drying is crushed using Universalpulverizer, powder
Broken machine sieve >=80 mesh obtains the fructus amomi polyoses extract powder of brown color, yield >=5.0% of fructus amomi polyoses extract, gained
Total starches >=15% in fructus amomi polyoses extract, moisture≤5.0%, 80 mesh percent of pass >=90%.
The volatile oil extractor is mentioned by the TL200 type volatile oil of Hangzhou San Te medication chemistry equipment Co., Ltd production
Take device.The volatile oil extractor is mainly made of three parts: first is that volatile oil extracting special oil-water separator, second is that Chinese medicine
Extractor, third is that automatic control cabinet.Volatile oil extracting special oil-water separator is connected on Chinese medicament extracting device by condenser, in
Two layers of medicine extractor point, internal layer are packed into medicinal material and water；Interlayer is heating layer, and vapor is passed through in interlayer and carries out heat temperature raising.
During the extraction process, after the liquid boiling in extractor, under the action of automatic control cabinet, realize that constant temperature extracts.Temperature can
With setting, adjusting and display, achieve the purpose that 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 can be realized side purification volatilization
Extracting solution is produced on oily side, and completes the device of separation and the collection of volatile oil and extracting solution, can be used.
Fructus amomi medicinal material during the preparation process, is crushed first, is broken villous amomum pericarp by the method for the present invention, convenient for subsequent
The dissolution of amomum fruit volatile oil and fructus amomi flavones, fructus amomi polysaccharide when heating extraction, then carries out in dedicated volatile oil extractor
Heating extraction extracts the flavones in fructus amomi, polysaccharide effective component while collecting amomum fruit volatile oil, obtains fructus amomi extraction
Fructus amomi extraction crude liquid is successively centrifuged, is concentrated, alcohol precipitation, is centrifuged again, obtaining alcohol precipitation supernatant and alcohol precipitation precipitating, alcohol by crude liquid
Heavy supernatant is spray-dried after being concentrated under reduced pressure, and produces fructus amomi chromocor extract, alcohol precipitation precipitating using heat-circulation oven or
Fructus amomi polyoses extract is produced in board-like vacuum desiccator drying, is reached in a technical process simultaneously by amomum fruit volatile oil, sand
The purpose that benevolence flavones, fructus amomi polysaccharide disposably extract maximizes the utilization rate of fructus amomi medicinal material, avoids the wasting of resources, warp
The method of the present invention is extracted, and the yield of amomum fruit volatile oil is up to 3.0% or more, and the yield of fructus amomi chromocor extract is up to 5.0% or more, fructus amomi
The yield of polyoses extract is up to 5.0% or more, and compared with traditional independent extraction single active ingredient, the yield of each product is differed
Less.
The method of the present invention simple process and low cost by being extracted to fructus amomi medicinal material using primary, while being obtained fructus amomi and waved
Hair oil, fructus amomi flavones, fructus amomi polyoses extract, comprehensively utilize fructus amomi medicinal material, obtained product can be applied to food,
The multiple fields such as drug, effectively reduce production cost, have significant economic benefit and social benefit.
Detailed description of the invention
Fig. 1 is technological process block-diagram of the invention.
Specific embodiment
Below to utilize fructus amomi to extract amomum fruit volatile oil, fructus amomi flavones in Jing Brand Bio-medicine Co., Ltd.'s actual production
And for the specific production process of fructus amomi polysaccharide, to explain in detail the present invention, but they are not limit the invention in any way,
The specific condition of production is as follows:
Embodiment 1
Referring to Fig. 1, a method of utilize fructus amomi to extract amomum fruit volatile oil, fructus amomi flavones, fructus amomi polysaccharide, including following steps
It is rapid:
(1) preparation of amomum fruit volatile oil: taking fructus amomi medicinal raw material 100kg, is added after being crushed fructus amomi medicinal material with crusher
In volatile oil extractor, the water of 1000L is added, impregnates 0.5 hour, heating extraction 5.0 hours, steam is condensed, collects
To amomum fruit volatile oil 3.0kg, the yield of amomum fruit volatile oil is 3.0%, and the relative density of gained amomum fruit volatile oil is 0.925, refractive power
Index is 1.499, and the content of Bronyl acetate is 454.5mg/ml；The volatile oil extractor is by Hangzhou San Te medication chemistry
The TL200 type volatile oil extractor of equipment Co., Ltd production；
(2) fructus amomi in step (1) volatile oil extractor the collection of amomum villosum extract: is extracted into crude liquid discharge, fructus amomi medicine
Slag discards；Fructus amomi is extracted into crude liquid and carries out high speed centrifugation with disc centrifuge, setting feeding temperature is 45 DEG C, and charging rate is
4000L/h, revolving speed 6000r/min are centrifuged 50min, and collecting centrifugate is amomum villosum extract, and the precipitating after centrifugation discards；
(3) it is concentrated: amomum villosum extract being concentrated under reduced pressure using dual-effect concentrator, control thickening temperature is 65 DEG C, dense
It is reduced to the raw material of fructus amomi containing 1g in every 1ml concentrate, obtains 100L concentrate；
(4) alcohol precipitation: the edible alcohol that 170L mass fraction is 95% is added in concentrate, makes the matter of ethyl alcohol in concentrate
Amount score reaches 60%, stirs evenly, and stands 12h and obtains alcohol precipitation solution；
(5) it is centrifuged: alcohol precipitation solution being separated using Horizontal helical type centrifuge, revolving speed 5500r/min respectively obtains alcohol
Heavy supernatant and alcohol precipitation precipitating；
(6) preparation of fructus amomi flavones: by alcohol precipitation supernatant made from step (5) using dual-effect concentrator depressurize it is dense
Ethyl alcohol is recycled in contracting, and control thickening temperature is 65 DEG C, and vacuum degree is -0.06MPa, is condensed into the medicinal extract that specific gravity is 1.08, will be concentrated
Medicinal extract afterwards is spray-dried, and control inlet air temperature is 190 DEG C, and leaving air temp is 90 DEG C, and dry powder is collected after spray drying and is obtained
To the fructus amomi chromocor extract powder 7.5kg of brown color, the yield of fructus amomi chromocor extract is 7.5%, gained fructus amomi extracting flavonoids
General flavone is 41.7% in object, moisture 3.5%, and 80 mesh percent of pass are 95%；
(7) preparation of fructus amomi polysaccharide: alcohol precipitation made from step (5) is precipitated, heat-circulation oven or board-like vacuum drying is added
In device, control drying temperature is dried at 60 DEG C, the material after drying is crushed using Universalpulverizer, pulverizer
Sieve >=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%, institute
Obtaining total starches in fructus amomi polyoses extract is 21.5%, moisture 3.7%, and 80 mesh percent of pass are 94%.
Embodiment 2
A method of amomum fruit volatile oil, fructus amomi flavones, fructus amomi polysaccharide being extracted using fructus amomi, is included the following steps:
(1) preparation of amomum fruit volatile oil: taking fructus amomi medicinal raw material 100kg, is added after being crushed fructus amomi medicinal material with crusher
In volatile oil extractor, the water of 1200L is added, impregnates 0.7 hour, heating extraction 5.5 hours, steam is condensed, collects
To amomum fruit volatile oil 3.1kg, the yield of amomum fruit volatile oil is 3.1%, and the relative density of gained amomum fruit volatile oil is 0.931, refractive power
Index is 1.502, and the content of Bronyl acetate is 428.7mg/ml；The volatile oil extractor is by Hangzhou San Te medication chemistry
The TL200 type volatile oil extractor of equipment Co., Ltd production；
(2) fructus amomi in step (1) volatile oil extractor the collection of amomum villosum extract: is extracted into crude liquid discharge, fructus amomi medicine
Slag discards；Fructus amomi is extracted into crude liquid and carries out high speed centrifugation with disc centrifuge, setting feeding temperature is 48 DEG C, and charging rate is
4500L/h, revolving speed 5000r/min are centrifuged 40min, and collecting centrifugate is amomum villosum extract, and the precipitating after centrifugation discards；
(3) it is concentrated: amomum villosum extract being concentrated under reduced pressure using dual-effect concentrator, control thickening temperature is 70 DEG C, dense
It is reduced to the raw material of fructus amomi containing 1g in every 1ml concentrate, obtains 100L concentrate；
(4) alcohol precipitation: the edible alcohol that 280L mass fraction is 95% is added in concentrate, makes the matter of ethyl alcohol in concentrate
Amount score reaches 70%, stirs evenly, and stands 12h and obtains alcohol precipitation solution；
(5) it is centrifuged: alcohol precipitation solution being separated using Horizontal helical type centrifuge, revolving speed 5300r/min respectively obtains alcohol
Heavy supernatant and alcohol precipitation precipitating；
(6) preparation of fructus amomi flavones: by alcohol precipitation supernatant made from step (5) using dual-effect concentrator depressurize it is dense
Ethyl alcohol is recycled in contracting, and control thickening temperature is 72 DEG C, vacuum degree 0.01MPa, is condensed into the medicinal extract that specific gravity is 1.10, will be concentrated
Medicinal extract afterwards is spray-dried, and control inlet air temperature is 195 DEG C, and leaving air temp is 95 DEG C, and dry powder is collected after spray drying and is obtained
To the fructus amomi chromocor extract powder 6.2kg of brown color, the yield of fructus amomi chromocor extract is 6.2%, gained fructus amomi extracting flavonoids
General flavone is 49% in object, moisture 3.1%, and 80 mesh percent of pass are 97%；
(7) preparation of fructus amomi polysaccharide: alcohol precipitation made from step (5) is precipitated, heat-circulation oven or board-like vacuum drying is added
In device, control drying temperature is dried at 70 DEG C, the material after drying is crushed using Universalpulverizer, pulverizer
Sieve >=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%, institute
Obtaining total starches in fructus amomi polyoses extract is 17.8%, moisture 2.9%, and 80 mesh percent of pass are 93%.
Embodiment 3
A method of amomum fruit volatile oil, fructus amomi flavones, fructus amomi polysaccharide being extracted using fructus amomi, is included the following steps:
(1) preparation of amomum fruit volatile oil: taking fructus amomi medicinal raw material 100kg, is added after being crushed fructus amomi medicinal material with crusher
In volatile oil extractor, the water of 1500L is added, impregnates 1.0 hours, heating extraction 6.0 hours, steam is condensed, collects
To amomum fruit volatile oil 3.0kg, the yield of amomum fruit volatile oil is 3.0%, and the relative density of gained amomum fruit volatile oil is 0.942, refractive power
Index is 1.501, and the content of Bronyl acetate is 445.4mg/ml；
(2) fructus amomi in step (1) volatile oil extractor the collection of amomum villosum extract: is extracted into crude liquid discharge, fructus amomi medicine
Slag discards；Fructus amomi is extracted into crude liquid and carries out high speed centrifugation with disc centrifuge, setting feeding temperature is 50 DEG C, and charging rate is
5000L/h, revolving speed 5000r/min are centrifuged 45min, and collecting centrifugate is amomum villosum extract, and the precipitating after centrifugation discards；
(3) it is concentrated: amomum villosum extract being concentrated under reduced pressure using dual-effect concentrator, control thickening temperature is 75 DEG C, dense
It is reduced to the raw material of fructus amomi containing 1g in every 1ml concentrate, obtains 100L concentrate；
(4) alcohol precipitation: the edible alcohol that 530L mass fraction is 95% is added in concentrate, makes the matter of ethyl alcohol in concentrate
Amount score reaches 80%, stirs evenly, and stands 12h and obtains alcohol precipitation solution；
(5) it is centrifuged: alcohol precipitation solution being separated using Horizontal helical type centrifuge, revolving speed 5000r/min respectively obtains alcohol
Heavy supernatant and alcohol precipitation precipitating；
(6) preparation of fructus amomi flavones: by alcohol precipitation supernatant made from step (5) using dual-effect concentrator depressurize it is dense
Ethyl alcohol is recycled in contracting, and control thickening temperature is 80 DEG C, vacuum degree 0.09MPa, is condensed into the medicinal extract that specific gravity is 1.12, will be concentrated
Medicinal extract afterwards is spray-dried, and control inlet air temperature is 200 DEG C, and leaving air temp is 100 DEG C, and dry powder is collected after spray drying and is obtained
To the fructus amomi chromocor extract powder 5.1kg of brown color, the yield of fructus amomi chromocor extract is 5.1%, gained fructus amomi extracting flavonoids
General flavone is 52.6% in object, moisture 2.8%, and 80 mesh percent of pass are 94%；
(7) preparation of fructus amomi polysaccharide: alcohol precipitation made from step (5) is precipitated, heat-circulation oven or board-like vacuum drying is added
In device, control drying temperature is dried at 80 DEG C, the material after drying is crushed using Universalpulverizer, pulverizer
Sieve >=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%, institute
Obtaining total starches in fructus amomi polyoses extract is 15.6%, moisture 3.0%, and 80 mesh percent of pass are 97%.
Claims (2)
1. a kind of method for extracting amomum fruit volatile oil, fructus amomi flavones and fructus amomi polysaccharide using fructus amomi, it is characterised in that including following
Step:
(1) preparation of amomum fruit volatile oil: taking fructus amomi medicinal raw material, and volatile oil extracting is added after being crushed fructus amomi medicinal material with crusher
In device, 10~15 times of material quality of water is added, impregnates 0.5~1.0 hour, extracts 5.0~6.0 hours, steam is carried out cold
It is solidifying, collect amomum fruit volatile oil, yield >=3.0% of amomum fruit volatile oil, the relative density of gained amomum fruit volatile oil is 0.918~
0.950, refraction index is 1.495~1.510, content >=400mg/ml of Bronyl acetate；
(2) collection of amomum villosum extract: the fructus amomi in step (1) volatile oil extractor is extracted into crude liquid discharge, the fructus amomi dregs of a decoction are abandoned
It goes；Fructus amomi is extracted into crude liquid and carries out high speed centrifugation with disc centrifuge, setting feeding temperature is 45~50 DEG C, charging rate
4000~5000L/h, revolving speed are 5000~6000r/min, are centrifuged 40~50min, and collecting centrifugate is amomum villosum extract, from
Precipitating after the heart discards；
(3) it is concentrated: amomum villosum extract being concentrated under reduced pressure using dual-effect concentrator, control thickening temperature is 65~75 DEG C, dense
It is reduced to the raw material of fructus amomi containing 1g in every 1ml concentrate；
(4) alcohol precipitation: the edible alcohol that 1.7~5.3 times of mass fractions of the volume of the concentrated liquid are 95% is added in concentrate, makes to be concentrated
The mass fraction of ethyl alcohol reaches 60~80% in liquid, stirs evenly, and stands 12h and obtains alcohol precipitation solution；
(5) it is centrifuged: alcohol precipitation solution being separated using Horizontal helical type centrifuge, revolving speed is 5000~5500r/min, is respectively obtained
Alcohol precipitation supernatant and alcohol precipitation precipitating；
(6) preparation of fructus amomi flavones: alcohol precipitation supernatant made from step (5) is concentrated under reduced pressure using dual-effect concentrator, is returned
Ethyl alcohol is received, control thickening temperature is 65~80 DEG C, and for vacuum degree between -0.06MPa~0.09MPa, being condensed into specific gravity is 1.08
Medicinal extract after concentration is spray-dried by~1.12 medicinal extract, and control inlet air temperature is 190~200 DEG C, leaving air temp 90
~100 DEG C, dry powder is collected after spray drying and obtains the fructus amomi chromocor extract powder of brown color, the yield of fructus amomi chromocor extract
>=5.0%, general flavone >=40% in gained fructus amomi chromocor extract, moisture≤5.0%, 80 mesh percent of pass >=90%；
(7) preparation of fructus amomi polysaccharide: alcohol precipitation made from step (5) is precipitated, heat-circulation oven or board-like vacuum desiccator is added
In, control drying temperature is dried at 60~80 DEG C, and the material after drying is crushed using Universalpulverizer, is crushed
Machine sieve >=80 mesh obtains the fructus amomi polyoses extract powder of brown color, yield >=5.0% of fructus amomi polyoses extract, gained sand
Total starches >=15% in benevolence polyoses extract, moisture≤5.0%, 80 mesh percent of pass >=90%.
2. a kind of method for extracting amomum fruit volatile oil, fructus amomi flavones and fructus amomi polysaccharide using fructus amomi according to claim 1,
It is characterized by: the volatile oil extractor is the TL200 type volatilization by the production of Hangzhou San Te medication chemistry equipment Co., Ltd
Oil extractor.
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| CN109134695B (en) * | 2018-08-08 | 2021-06-08 | 劲牌生物医药有限公司 | Alcohol-soluble beta-glucan extract, preparation method and application thereof, and health-care wine |
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| CN105169203A (en) * | 2015-09-25 | 2015-12-23 | 云南中医学院 | Fructus amomi extract and application thereof |
| CN105362311A (en) * | 2015-11-23 | 2016-03-02 | 安徽科技学院 | Method for extracting and separating volatile oil, flavone and polysaccharide of abelmoschus manihot flowers |
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| CN105169203A (en) * | 2015-09-25 | 2015-12-23 | 云南中医学院 | Fructus amomi extract and application thereof |
| CN105362311A (en) * | 2015-11-23 | 2016-03-02 | 安徽科技学院 | Method for extracting and separating volatile oil, flavone and polysaccharide of abelmoschus manihot flowers |
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