CN100431551C - Method for extracting effect composition from pilose antler using overcritical extraction equipment - Google Patents
Method for extracting effect composition from pilose antler using overcritical extraction equipment Download PDFInfo
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- CN100431551C CN100431551C CNB2005100172155A CN200510017215A CN100431551C CN 100431551 C CN100431551 C CN 100431551C CN B2005100172155 A CNB2005100172155 A CN B2005100172155A CN 200510017215 A CN200510017215 A CN 200510017215A CN 100431551 C CN100431551 C CN 100431551C
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- 238000000605 extraction Methods 0.000 title claims description 30
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- 230000000694 effects Effects 0.000 title description 3
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- 239000007788 liquid Substances 0.000 claims abstract 2
- 238000000926 separation method Methods 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 9
- 238000000194 supercritical-fluid extraction Methods 0.000 claims description 9
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- 150000001413 amino acids Chemical class 0.000 description 5
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- 108090000723 Insulin-Like Growth Factor I Proteins 0.000 description 3
- 102000013275 Somatomedins Human genes 0.000 description 3
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- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 229920002683 Glycosaminoglycan Polymers 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
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- 229920002472 Starch Polymers 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
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- 239000013543 active substance Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 235000013305 food Nutrition 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000007902 hard capsule Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
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- 229910052698 phosphorus Inorganic materials 0.000 description 1
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- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 150000003180 prostaglandins Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000003488 releasing hormone Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 235000019515 salmon Nutrition 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007901 soft capsule Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 230000003637 steroidlike Effects 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
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- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
A process for extracting the active components from pilose antler by use of supercritical extracting apparatus includes such steps as washing fresh pilose antler, slicing or breaking, supercritical CO2 extracting three times, collecting the liquid extract, vacuum drying, and pulverizing.
Description
Technical field
The present invention relates to a kind of deep working method of velvet product, a kind of specifically process of from Cornu Cervi Pantotrichum, extracting active ingredient (Cornu Cervi Pantotrichum element) with supercritical extraction equipment.
Background technology
According to record, China be the earliest with Cornu Cervi Pantotrichum as medicinal country, so far have the history in more than 2,000 year, why lasting Cornu Cervi Pantotrichum is as a kind of Chinese medicine, be because it has due to unique pharmacological function, Main Ingredients and Appearance in the Cornu Cervi Pantotrichum: Organic substance 61.19%---63.44%, inorganic matter 24.45-27.22%, moisture 11.59---12.11%.Inorganic composition mainly is calcium, phosphorus, aluminum, magnesium, silver, copper, zinc, barium, ferrum, manganese, stannum, silicon, strontium, lead, cobalt, thallium, vanadium, sodium, zirconium etc.Organic component is the main matter basis that Cornu Cervi Pantotrichum has the special pharmacological effect, is divided into water solublity, fat-soluble and insoluble substance according to its dissolved substance: mainly comprise 19 seed amino acids, polypeptide, protein in the water-soluble substances; Mucopolysaccharide, mucin, amidohexose and glucose.Liposoluble substance mainly is phospholipid, steroidal compounds, fatty acid, neutral fat, vitamins and prostaglandin etc.; Insoluble substance mainly comprises materials such as scleroprotein and collagenic protein.Except that containing above various active physiology composition, also contain material IGF-1 (insulin like growth factor), HGH (human body HGH) GHRF-6 (growth promotion releasing factor) of high-grade anti-human senility etc. in the modern biotechnology discovery Cornu Cervi Pantotrichum.Discover that the IGF-1 in the Cornu Cervi Pantotrichum, HGH, GHRF-6 etc. are the highest aminoacid materials of anti-human senility.The present invention uses modern extraction equipment the active ingredient of Cornu Cervi Pantotrichum---and the Cornu Cervi Pantotrichum element extracts, and makes health food, the functional food of difference in functionality, for people provide brand-new health-care good product, the economic benefit that enterprise is obtained.
Known water extraction and alcohol extraction are followed the example of, and active ingredient content is low in the Cornu Cervi Pantotrichum extract of acquisition, and also have many materials that are difficult for being absorbed by the body to be obtained through refining out, as anaphylactogens such as cellulose, soluble starches; Inner Mongol mahatma's biotechnology company extracts Cornu Cervi Pantotrichum element its 18 seed amino acid after testing with the ultrasound wave water extraction, and total content is 7760.67mg/100g; It is 70.41% that 28 kinds of fatty acids extract total amount; SOD is 510 μ/ml; And 18 seed amino acid total contents are 70 in the Cornu Cervi Pantotrichum element that we extract with supercritical extraction, and 396.47mg/100g is 9 times of ultrasonic extraction; The content of 28 kinds of fatty acids reaches 98.97%, increases yield 28.56% than ultrasonic extraction; SOD is 1025 μ/ml, is 2 times of supercritical ultrasonics technology.
Summary of the invention
The objective of the invention is to be solve to adopt water extraction and alcohol extraction to follow the example of to extract in the Cornu Cervi Pantotrichum effective ingredient yield low, the deficiency that active constituent content such as aminoacid, fatty acid is low provides the high supercritical extraction equipment of using of active constituent content of a kind of yield height, extraction to extract the process of active ingredient from Cornu Cervi Pantotrichum.
The object of the present invention is achieved like this,
The present invention adopts CO
2The liquid phase supercritical extraction process prepares and gets, and its concrete processing step is:
1., bright Cornu Cervi Pantotrichum (band blood) is cleaned up, the airing surface moisture is cut into lamellar or is ground into graininess standby with cutting knife or pulverizer;
2., single extraction: with the material of the above-mentioned pulverizing extraction kettle of packing into, extraction kettle, separation reactor I, separation reactor I I are given heating, design temperature is extraction temperature 45-50 ℃, and the separation reactor I temperature is 40-45 ℃, and separation reactor I I temperature is 30-35 ℃, opens C O
2Gas cylinder, flow-control adds 10-15kg at every kg Cornu Cervi Pantotrichum, simultaneously whole system is pressurizeed, when extracting pressure reaches 28-33MPa, separation reactor I pressure reaches 5.5-6.5Mpa, closes gas cylinder when separation reactor I I pressure reaches 4.5-5.5Mpa, and it is 90-120 minute that the extraction time is controlled at 1.5-2 hour, decompress(ion) is also regained gas, and the extract of withdrawal presents light yellow;
3., reextraction, to add dehydrated alcohol after the filter residue and drying behind the single extraction, extracting pressure, temperature, separating pressure, temperature are with above-mentioned parameter in 2., the extraction time is controlled in 2 hours scopes, decompress(ion) is regained extract, with ethanol evaporation, get the brownish red oil-like extracts with rotary evaporator;
4., extract for three times: will add the water of 10 times of weight after the reextraction after-filtration melt cinder drying, extract for continuous three times with the ultrasonic extraction machine, temperature is controlled between 40-45 ℃, each 30 minutes of time, gets the brown jelly;
5., above-mentioned 2., 3., the material uniform mixing that 4. extracts in three steps gets product of the present invention (Cornu Cervi Pantotrichum element) mother solution, after vacuum drying is pulverized solid product of the present invention (Cornu Cervi Pantotrichum element).
Supercritical extraction main feature of the present invention: the one, pure physics mode extracts active substance in the Cornu Cervi Pantotrichum, and IGF, HGH, GHRF-6 are retained; The 2nd, extract yield is higher than that water is carried, alcohol extraction or ultrasonic extraction method; The 3rd, extractant CO
2Stable performance, the price appropriateness, extraction cost is lower; The 4th, do not add any chemical addition agent, the Cornu Cervi Pantotrichum element of obtaining through refining is the pure natural product.
Utilize the special pharmacological effect of product of the present invention (Cornu Cervi Pantotrichum element) and, can be made into the Cornu Cervi Pantotrichum prime system row function food product of pure natural, health foods such as the plain hard capsule of Cornu Cervi Pantotrichum, Cornu Cervi Pantotrichum cellulose soft capsules, the plain drop pill of Cornu Cervi Pantotrichum the special curing effect of human body skin; Or, make Cornu Cervi Pantotrichum prime system row cosmetics based on the Cornu Cervi Pantotrichum element.
Description of drawings
Fig. 1 is for extracting preparation technology's flow chart of active ingredient in the Cornu Cervi Pantotrichum with supercritical extraction equipment.
The specific embodiment
1, gets Cornu Cervi Pantotrichum (band blood) 250g and purify the back cut into serving pieces.
2, extraction for the first time: the material of cut into serving pieces is added in the extraction kettle.With extraction kettle, separation reactor I, separation reactor I I give heating, and design temperature is 50 ℃ of extraction temperature; The separation reactor I temperature is that 45 ℃, separation reactor I I temperature are 35 ℃, opens CO
2Gas cylinder, flow-control adds 12.5kg/h at every kg Cornu Cervi Pantotrichum, simultaneously system is pressurizeed, when extracting pressure reaches 28Mpa, close gas cylinder when separation reactor I pressure 6Mpa, separation reactor I I pressure 5Mpa, constant temperature and pressure extraction 2 hours, decompress(ion) also reclaims gas, take out light yellowly from separating still, it is 15% that grease extract 37.5g extracts yield for the first time.
3, extraction for the second time: the dehydrated alcohol that adds 2 times of amounts after the bits drying after the extracting solution filter for the first time, extraction temperature, pressure, the time repeats said procedure, after ethanol in the extract evaporated with rotary evaporator (productions in single-action or double effect evaporator), must 3.75g salmon pink grease.
4, extracting for the third time, is 100g with the dry weighing of bits after the extract filter second time, adds 10 times in water and circulates with ultrasound wave and extract for three times, and the temperature of extraction is 42 ℃, and the time is 28 minutes, and extracting solution weighing after drying gets brown jelly 23.75g.
5, get the plain 65g of Cornu Cervi Pantotrichum extract Cornu Cervi Pantotrichum in above-mentioned 2,3,4 steps, total recovery is 65g/250g=26%.
Claims (1)
1, a kind of method with active ingredient in the supercritical extraction equipment extraction Cornu Cervi Pantotrichum, it is characterized in that: this method is to adopt CO
2The liquid phase supercritical extraction process prepares and gets, and its concrete processing step is:
1., bright Cornu Cervi Pantotrichum is cleaned up, the airing surface moisture is cut into lamellar or is ground into graininess standby with cutting knife or pulverizer;
2., single extraction: with the material of the above-mentioned pulverizing extraction kettle of packing into, extraction kettle, separation reactor I, separation reactor I I are given heating, design temperature is extraction temperature 45-50 ℃, and the separation reactor I temperature is 40-45 ℃, and separation reactor I I temperature is 30-35 ℃, opens CO
2Gas cylinder, flow-control adds 10-15kg at every kg Cornu Cervi Pantotrichum, simultaneously whole system is pressurizeed, when extracting pressure reaches 28-33MPa, separation reactor I pressure reaches 5.5-6.5Mpa, closes gas cylinder when separation reactor I I pressure reaches 4.5-5.5Mpa, and it is 90-120 minute that the extraction time is controlled at 1.5-2 hour, decompress(ion) is also regained gas, and the extract of withdrawal presents light yellow;
3., reextraction, to add dehydrated alcohol after the filter residue and drying behind the single extraction, extracting pressure, temperature, separating pressure, temperature are with above-mentioned parameter in 2., the extraction time is controlled in 2 hours scopes, decompress(ion) is regained extract, with ethanol evaporation, get the brownish red oil-like extracts with rotary evaporator;
4., extract for three times: will add the water of 10 times of weight after the reextraction after-filtration melt cinder drying, extract for continuous three times with the ultrasonic extraction machine, temperature is controlled between 40-45 ℃, each 30 minutes of time, gets the brown jelly;
5., above-mentioned 2., 3., the material uniform mixing that 4. extracts in three steps gets product mother liquid, after vacuum drying is pulverized solid product.
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| CNB2005100172155A CN100431551C (en) | 2005-10-24 | 2005-10-24 | Method for extracting effect composition from pilose antler using overcritical extraction equipment |
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| CNB2005100172155A CN100431551C (en) | 2005-10-24 | 2005-10-24 | Method for extracting effect composition from pilose antler using overcritical extraction equipment |
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| CN100431551C true CN100431551C (en) | 2008-11-12 |
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| CN101920128B (en) * | 2010-08-06 | 2013-01-02 | 河南科技大学 | Method for obtaining extractive by solvent extraction method under conditions of pressurization and ultrasonic irradiation |
| CN102058082B (en) * | 2010-11-22 | 2012-10-03 | 晨光生物科技集团股份有限公司 | Efficient extraction and separation technology for effective ingredients of peppers |
| CN104887706A (en) * | 2015-06-10 | 2015-09-09 | 吉林大学 | Concentrated coronet granules and preparation method thereof |
| CN112755053A (en) * | 2019-11-05 | 2021-05-07 | 湖南许丰现代农业股份有限公司 | Processing technology of traditional Chinese medicine tianlong |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1481815A (en) * | 2003-07-24 | 2004-03-17 | 白秀娟 | Supercritical CO2 method of preparing antler extract product |
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| CN1481815A (en) * | 2003-07-24 | 2004-03-17 | 白秀娟 | Supercritical CO2 method of preparing antler extract product |
Non-Patent Citations (2)
| Title |
|---|
| 鹿茸提取物体外抗氧化作用. 陈晓光.中药材，第26卷第10期. 2003 |
| 鹿茸提取物体外抗氧化作用. 陈晓光.中药材，第26卷第10期. 2003 * |
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Effective date of registration: 20151012 Address after: 130700 Jilin Province Siping City Yitong Manchu Autonomous County Dongying Jiyun Deer Industry Development Zone No. 666 Patentee after: Li Xuefeng Address before: 130700 Dongying Development Zone, Yitong Town, Yitong Manchu Autonomous County, Jilin Patentee before: Jiyun Deer Industrial Development Co., Ltd., Yitong Man Nationality Autonomous C |
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