CN1273205C - Method for extracting effective constituent from natural medicinal plant by double frequency ultrasonic alternative reinforcing supercritical fluid extraction device - Google Patents
Method for extracting effective constituent from natural medicinal plant by double frequency ultrasonic alternative reinforcing supercritical fluid extraction device Download PDFInfo
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- CN1273205C CN1273205C CN 200310117437 CN200310117437A CN1273205C CN 1273205 C CN1273205 C CN 1273205C CN 200310117437 CN200310117437 CN 200310117437 CN 200310117437 A CN200310117437 A CN 200310117437A CN 1273205 C CN1273205 C CN 1273205C
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- supercritical fluid
- extraction
- medicinal plant
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 15
- 239000000470 constituent Substances 0.000 title 1
- 230000003014 reinforcing effect Effects 0.000 title 1
- 238000000605 extraction Methods 0.000 claims abstract description 40
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 239000004480 active ingredient Substances 0.000 claims abstract description 16
- 239000012530 fluid Substances 0.000 claims abstract description 13
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 238000010298 pulverizing process Methods 0.000 claims abstract description 3
- 239000000284 extract Substances 0.000 claims description 15
- 238000002604 ultrasonography Methods 0.000 claims description 13
- 241000196324 Embryophyta Species 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000003814 drug Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 241000425037 Toona sinensis Species 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 241000209205 Coix Species 0.000 claims description 2
- 241000195493 Cryptophyta Species 0.000 claims description 2
- 241001529246 Platymiscium Species 0.000 claims description 2
- 229940079593 drug Drugs 0.000 claims description 2
- 238000000638 solvent extraction Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000005728 strengthening Methods 0.000 abstract 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 235000020673 eicosapentaenoic acid Nutrition 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229930003944 flavone Natural products 0.000 description 4
- 150000002213 flavones Chemical class 0.000 description 4
- 235000011949 flavones Nutrition 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 244000077995 Coix lacryma jobi Species 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 240000004859 Gamochaeta purpurea Species 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- JAZBEHYOTPTENJ-JLNKQSITSA-N all-cis-5,8,11,14,17-icosapentaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O JAZBEHYOTPTENJ-JLNKQSITSA-N 0.000 description 1
- 230000002567 autonomic effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960005135 eicosapentaenoic acid Drugs 0.000 description 1
- JAZBEHYOTPTENJ-UHFFFAOYSA-N eicosapentaenoic acid Natural products CCC=CCC=CCC=CCC=CCC=CCCCC(O)=O JAZBEHYOTPTENJ-UHFFFAOYSA-N 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention relates to a method for extracting active ingredients of natural medicinal plants by alternately strengthening supercritical fluid through double-frequency ultrasonic waves. The present invention orderly comprises the following steps that a. raw materials are preprocessed, including impurity removal, dryness and pulverization of the raw materials, and the raw materials are sieved by a screen of 10 to 120 meshes; b. the raw materials are extracted and separated by an extraction device by alternately strengthening supercritical fluid through double-frequency ultrasonic waves, the frequency of the double-frequency ultrasonic wave is from 16kHz to 100kHz, the power is from 0 to 1000W, the sound intensity is from 0.2 to 1500 W/cm, and the irradiation time is from 2 to 5 hours. Compared with the existing solvent extraction method and the supercritical fluid extraction method, the method has the advantages of high extraction rate, short time, low energy consumption, no pollution, simple devices, difficult damage to active ingredients, and easy popularization and application.
Description
Technical field
The present invention relates to the natural medicinal plant extraction of effective components, refer to adopt double-frequency ultrasound to replace the method for enhanced supercritical fluid extraction natural medicinal plant active ingredient especially.
Background technology
China is the profuse country of autonomic drug resource in the world, but because the hysteresis of production method causes product quality to compare the bigger gap of existence with world advanced person's medicine company enterprise, has restricted the process of China's modernization of Chinese medicine greatly.China's Chinese medicine general export ratio only accounts for 1% of world's medicine total sales volume.Tradition natural medicinal plant extraction of effective components generally is a solvent extraction method.It is residual few that this method has extract active ingredient, and extract quality is good, and processing cost is low, extracts in the airtight equipment of being everlasting and carry out, and produce and easily realize serialization, thereby labour intensity is low, and working condition is good.But it is inflammable and explosive substances that there are a lot of solvents in solvent extraction method, and solvent consumption is big, has certain residual quantity in extract, and majority has certain toxicity.Occur supercritical liquid extraction technique in recent ten years, supercritical fluid extraction is compared with traditional solvent extraction has the yield height, and with short production cycle, active ingredient is not destroyed, no solvent residue or residual quantity advantage seldom.But the pressure ratio of supercritical fluid extraction is higher simultaneously, equipment is required high; When adopting single extractant, dissolubility, selectivity are not enough sometimes, and extractability is little; Need higher system pressure during extraction and increase the solvent cycle-index just can obtain enough extraction quantities, be difficult to extract efficiently object; Equipment energy consumption is also bigger in the operating process.
Summary of the invention
For solving the existence deficiency of above-mentioned natural medicinal plant extracts active ingredients technology, the object of the invention provides a kind of new extraction natural medicinal plant active ingredient method, the ultrasonic wave that this method can be launched two kinds of different frequencies combines with supercritical liquid extraction technique to act on simultaneously and treats extract, improve extraction efficiency, reduce extracting pressure and extraction temperature, shorten the extraction time, reduce the consumption of entrainer, natural medicinal plant active ingredient is difficult for destroyed.
Method of the present invention is made up of two steps:
A. the pre-treatment of raw material comprises removal of impurities, drying, the pulverizing of raw material, sieves, and choosing particle size is 10～120 purpose raw materials.
B. replace enhanced supercritical fluid extraction device with double-frequency ultrasound raw material is carried out extract and separate.
Describe each step of the present invention below in detail:
1. the specific operation process of raw material pre-treatment is: extracting used raw material is Meliaceae Chinese toon platymiscium class, Coix or marine algae.Fresh or dry raw material need be removed impurity and other foreign matters such as rubble, sand and iron block, need pass through drying and dehydrating for fresh raw material, requires its water content below 2%.Raw material for drying directly carries out grinding and sieving, and choosing particle size is 10～120 purpose raw materials.
2. double-frequency ultrasound alternately hands over the detailed process of enhanced supercritical fluid extraction natural medicinal plant active ingredient to be: choosing particle diameter is that 10～120 purpose raw materials are put into extraction kettle, the raw material inventory is the capacity of 50～200g material/L extractor, adopts double-frequency ultrasound to replace enhanced supercritical CO
2Extraction, the double-frequency ultrasound wave frequency is 16kHz～100kHz, and power is 0～1000W, and the sound intensity is 0.2～1500W/cm
2, exposure time is 2～5 hours; Extraction temperature is 32-70 ℃, and extracting pressure is 10-60MPa, and extraction is to being 2-5 hour, and the extraction fluid flow is 2.0～50L/h, and the entrainer consumption of ethanol is 0～100ml/100g.
Advantage of the present invention:
1. the present invention combines double-frequency ultrasound and supercritical liquid extraction technique, can obviously reduce the pressure and the extraction temperature of supercritical fluid extraction, shortens the extraction time, reduces the consumption of entrainer.
2. the present invention compares with supercritical fluid extraction, and its product extraction yield improves 10～300%.
3. the good product quality of gained of the present invention, active ingredient is difficult for destroyed, the purity height, no solvent residue, pollution-free.
4. technology of the present invention is simple, and energy consumption is low, and equipment is simple, and cost is low, is easy to apply.
The specific embodiment
The invention will be further described below in conjunction with case study on implementation.Below the raw material that is taken by weighing in the case of Shi Shiing all is the dried powders that make by the following method: fresh or dry raw material needs distiller's yeast to remove impurity and other foreign matters such as rubble, sand and iron block, need pass through drying and dehydrating for fresh raw material, require its water content below 2%, raw material for drying directly carries out grinding and sieving, and choosing particle size is 10～120 purpose raw materials.The raw material inventory is the capacity of 50～200g material/L extractor.
Case study on implementation 1: the extraction of flavones in the Chinese Toon Leaves
Extraction conditions: the extraction frequency is 16kHz and 64kHz, and power is 300W, and the sound intensity is 20W/cm
2, the double frequency alternately irradiated time respectively is 1 hour, and irradiation total time is 2 hours, and supercritical fluid is a carbon dioxide, and extraction temperature is 60 ℃, and extracting pressure is 50MPa, and the extraction time is 2 hours, and the extraction fluid flow is 8L/h, the entrainer consumption is 90ml ethanol/100gCO
2
| Title | Weight (g) | The content of flavones (mg/g) | Flavones total amount (g) | The recovery rate of flavones (%) |
| Chinese Toon Leaves | 100 | 71.5 | 7.15 | |
| Extract remainder | 82.6 | 36.6 | 3.02 | |
| Extract | 16.5 | 245.5 | 4.05 | 56.7 |
Case study on implementation 2: from marine alga, extract eicosapentaenoic acid (EPA)
Extraction conditions: the extraction frequency is 34kHz and 95kHz, and power is 900W, and the sound intensity is 1400W/cm
2, the double frequency alternately irradiated time respectively is 2 hours, and irradiation total time is 4 hours, and supercritical fluid is a carbon dioxide, and extraction temperature is 45 ℃, and extracting pressure is 15MPa, and the extraction time is 4 hours, and the extraction fluid flow is 46L/h, the entrainer consumption is 5ml ethanol/100gCO
2
| Title | Weight (g) | The content of EPA (mg/g) | EPA total amount (g) | The recovery rate of EPA (%) |
| Marine alga | 100 | 246 | 24.6 | |
| Extract remainder | 47.6 | 16.8 | 0.8 | |
| Extract | 51.3 | 450.3 | 23.1 | 96.7 |
Case study on implementation 3: from coix seed, extract coix seed oil (CLSO)
Extraction conditions: the extraction frequency is 42kHz and 69kHz, and power is 500W, and the sound intensity is 600W/cm
2, the double frequency alternately irradiated time respectively is 1.5 hours, irradiation total time is 3 hours, supercritical fluid is a carbon dioxide, and extraction temperature is 32 ℃, and extracting pressure is 35MPa, the extraction time is 3 hours, and the extraction fluid flow is 26L/h, and the entrainer consumption is 23ml ethanol/100gCO
2
| Title | Weight (g) | The content of CLSO (mg/g) | CLSO total amount (g) | The recovery rate of CLSO (%) |
| Heart of a lotus seed benevolence | 100 | 108 | 10.8 | |
| Extract remainder | 70.8 | 7.1 | 0.5 | |
| Extract | 38.3 | 258.4 | 9.9 | 98.9 |
Claims (4)
1. a double-frequency ultrasound replaces the method for enhanced supercritical fluid extraction natural medicinal plant active ingredient, it is characterized in that described double-frequency ultrasound wave frequency is 16～100kHz, and power is 0～1000W, and the sound intensity is 0.2～1500W/cm
2, exposure time is 2～5 hours, and the mode of action is the ultrasonic wave alternating action of two kinds of different frequencies, and supercritical fluid is a supercritical CO
2Fluid, this method comprises the steps: successively
A. raw material sieves by 10～120 purposes through dry after the removal of impurities, pulverizing;
B. replace enhanced supercritical fluid extraction device with double-frequency ultrasound raw material is carried out extract and separate drug active ingredient.
2. replace the method for enhanced supercritical fluid extraction natural medicinal plant active ingredient by the described double-frequency ultrasound of claim 1, the extraction temperature that it is characterized in that described supercritical fluid is 32～70 ℃, extracting pressure is 10～60MPa, the extraction time is 2～5 hours, the extraction fluid flow is 2.0～50L/h, and the entrainer consumption of ethanol is 0～100ml ethanol/100gCO
2
3. replace the method for enhanced supercritical fluid extraction natural medicinal plant active ingredient by the described double-frequency ultrasound of claim 1, the particle diameter that it is characterized in that raw material is 10～120 orders, and inventory is the capacity of 50～200g material/L extractor.
4. replace the method for enhanced supercritical fluid extraction natural medicinal plant active ingredient by the described double-frequency ultrasound of claim 1, it is characterized in that natural medicinal plant comprises Meliaceae Chinese toon platymiscium class, Coix and marine algae.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310117437 CN1273205C (en) | 2003-12-19 | 2003-12-19 | Method for extracting effective constituent from natural medicinal plant by double frequency ultrasonic alternative reinforcing supercritical fluid extraction device |
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| CN 200310117437 CN1273205C (en) | 2003-12-19 | 2003-12-19 | Method for extracting effective constituent from natural medicinal plant by double frequency ultrasonic alternative reinforcing supercritical fluid extraction device |
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| CN1628888A CN1628888A (en) | 2005-06-22 |
| CN1273205C true CN1273205C (en) | 2006-09-06 |
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| CN 200310117437 Expired - Fee Related CN1273205C (en) | 2003-12-19 | 2003-12-19 | Method for extracting effective constituent from natural medicinal plant by double frequency ultrasonic alternative reinforcing supercritical fluid extraction device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108210383A (en) * | 2017-11-06 | 2018-06-29 | 朱浩奇 | A kind of preparation method of Herba Euphrasiae Regelii extract used for cosmetic |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102860538A (en) * | 2012-09-03 | 2013-01-09 | 江苏大学 | Alternate double-frequency countercurrent ultrasonic-assisted simultaneous extraction method for seaweed protein and polysaccharide mixed product |
| CN105767807A (en) * | 2016-03-23 | 2016-07-20 | 合肥中科玛卡生物技术有限公司 | Maca fruit and vegetable drink and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108210383A (en) * | 2017-11-06 | 2018-06-29 | 朱浩奇 | A kind of preparation method of Herba Euphrasiae Regelii extract used for cosmetic |
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| CN1628888A (en) | 2005-06-22 |
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Guangdong Jiaduobao Drink&Food Co., Ltd. Assignor: South China University of Technology Contract fulfillment period: 2007.10.20 to 2013.12.31 contract change Contract record no.: 2008440000264 Denomination of invention: Method for extracting effective constituent from natural medicinal plant by double frequency ultrasonic alternative reinforcing supercritical fluid extraction device Granted publication date: 20060906 License type: Exclusive license Record date: 2008.10.9 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.10.20 TO 2013.12.31; CHANGE OF CONTRACT Name of requester: GUANGDONG JIADUOBAO BEVERAGES AND FOODSTUFFS CO., Effective date: 20081009 |
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| EC01 | Cancellation of recordation of patent licensing contract |
Assignee: Guangdong Jiaduobao Drink&Food Co., Ltd. Assignor: South China University of Technology Contract record no.: 2008440000264 Date of cancellation: 20150114 |
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Application publication date: 20050622 Assignee: HEFEI USTC MACA BIOTECHNOLOGY CO., LTD. Assignor: South China University of Technology Contract record no.: 2015340000002 Denomination of invention: Method for extracting effective constituent from natural medicinal plant by double frequency ultrasonic alternative reinforcing supercritical fluid extraction device Granted publication date: 20060906 License type: Exclusive License Record date: 20150119 |
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Granted publication date: 20060906 Termination date: 20161219 |
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