CN103110678B - A kind of preparation method of saponin(e - Google Patents
A kind of preparation method of saponin(e Download PDFInfo
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- CN103110678B CN103110678B CN201310062109.3A CN201310062109A CN103110678B CN 103110678 B CN103110678 B CN 103110678B CN 201310062109 A CN201310062109 A CN 201310062109A CN 103110678 B CN103110678 B CN 103110678B
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- extractor
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- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 15
- 229930182490 saponin Natural products 0.000 title claims abstract description 15
- 150000007949 saponins Chemical class 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000006260 foam Substances 0.000 claims abstract description 23
- 238000000605 extraction Methods 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 229930182494 ginsenoside Natural products 0.000 claims abstract description 12
- 229940089161 ginsenoside Drugs 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000284 extract Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 230000005587 bubbling Effects 0.000 abstract description 2
- 238000005187 foaming Methods 0.000 abstract 1
- 230000001151 other effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 18
- 230000008569 process Effects 0.000 description 9
- 238000005265 energy consumption Methods 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 241000208340 Araliaceae Species 0.000 description 6
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 6
- 235000003140 Panax quinquefolius Nutrition 0.000 description 6
- 239000003814 drug Substances 0.000 description 6
- 238000005485 electric heating Methods 0.000 description 6
- 235000008434 ginseng Nutrition 0.000 description 6
- 238000011161 development Methods 0.000 description 4
- 239000008213 purified water Substances 0.000 description 4
- 238000010923 batch production Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000419 plant extract Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241001037751 Fusarium oxysporum f. sp. vanillae Species 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Steroid Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
A kind of preparation method of saponin(e, comprising: (1) root, stem, leaf or flower are placed in extractor, solvent is added and carries out dynamic outer circulating extracting；(2) it is bubbled on extracting circuit with bubbling device, and foam is drawn, is collected；(3) foam collected is abolished with foam separator, becomes highly concentrated total saposins liquid；(4) it carries out conventional concentration, be dried.The present invention is easy the characteristic of blistering according to ginsenoside, and the disadvantage of this traditional handicraft is switched to advantage, overcomes the existing preparation process effective component rate of transform low, step is various, the problems such as concentration is difficult, and the operation cycle is long, at high cost, make full use of dynamic outer circulating extracting feature and saponin(e characteristic easy to foaming, it is rationally designed, extraction process while isolated highly concentrated total saposins liquid reach simplified processing step, shorten the production cycle, improves yield and other effects.
Description
Technical field
The present invention relates to a kind of preparation methods of saponin(e.
Background technique
At present general ginsenoside prepare most common method be water mention, be concentrated, alcohol precipitation, concentration, drying process, this method water mentions
The concentration operation difficulty of liquid is big, and entire processing step is cumbersome, and the production cycle is long, and the equipment needed is more, and energy consumption is high, effective component
Loss is big, and purity is low, and production cost is higher, and largely both dangerous or not environmentally using alcohol.
Also water mentions, resin separation purification, concentration, drying process, this technological advantage is that ginsenoside purity is higher, but lacks
Point is largely using resin and alcohol, and cost is very high, and more demanding to the operation of worker, safety and environmental protection are poor.
The contradiction of the contradiction of plant extracts industry development and pollution, high investment and low output is compeled to be solved, utilizes substance
The operating feature of characteristic combination existing device carries out reasonably optimizing, combination, is the energy saving, excellent of solution plant extracts industry development
The feasible thinking of the problems such as matter, environmental protection and sustainable development.
Summary of the invention
Technical problem to be solved by the present invention lies in overcoming, conventional preparation techniques step is more, and concentration is difficult, production week
The technical problems such as the phase is long, and the effective component rate of transform is low, and energy consumption is high, and alcohol is largely used are easy the spy of blistering according to ginsenoside
Property, by this it has been generally acknowledged that the shortcomings that switch to advantage, dynamic outer circulating extracting is combined together with Bubble fractionation, reduce concentration,
Wine is heavy, reaches simplified processing step, shortens the production cycle, reduce energy consumption, improves effective component yield, avoid using wine
The effect of the organic solvents such as essence has significant contribution in simplified operation, energy conservation and environmental protection, production safety, save the cost.
The present invention provides a kind of preparation methods of saponin(e, comprise the following specific steps that:
(1) medicinal material is placed in extractor, water, or the ethanol solution lower than 50 degree is added, in 80 ~ 100 DEG C of progress dynamics
Outer circulating extracting, for volume 2.5L extractor, circulation rate is 1 ~ 10L/h, and the extractor of other volumes is with linear velocity phase
Deng principle change uninterrupted, extraction time be 2 ~ 4h；
(2) simultaneously or after extracting, sparger is bubbled, and capacity is 0.5 ~ 5L/min, by the body of sparger
Product makes foam from spilling suitable for reading, collects along pipeline and enter foam separator than amplification, and the liquid not blistered in sparger
Again it flows back to and participates in extracting in extractor.
(3) foam separator revolving speed is that highly concentrated total saposins extracting solution is obtained after foam fraction factor greater than 800 turns/min.
In the present invention, the medicinal material is root, stem, leaf and/or flower.
In the present invention, the saponin(e is high saponin content medicinal material.Preferably, the saponin(e is ginsenoside.
In the present invention, the method for the Extraction solvent is to put water to the ethanol solution of 30-70wt%, Extracting temperature 80 ~
100 DEG C, extraction time is 2 ~ 4h, and in the extractor that volume is 2.5L, liquid circulation velocity is 1 ~ 10L/h, Froth centrifugation
Revolving speed is not less than 800 turns/min, and the capacity of bubbler is 0.5 ~ 5L/min.Preferably, the concentration of the ethanol solution is
50wt%。
The technical effects of the invention are that:
1) present invention is that as long as doing lesser change to existing equipment the party can be realized in the characteristic for making full use of saponin(e
The preparation cost of ginsenoside is greatly reduced in method, and more environment-friendly and safer；
2) simplify processing step, shorten the production cycle: this technique extraction process and ginsenoside enrichment process carry out simultaneously,
Highly concentrated general ginsenoside liquid is made, the amount of concentration is greatly reduced, and eliminates the steps such as traditional filtering, the heavy, refrigeration of wine
Suddenly；
3) energy saving: the maximum operating unit of energy consumption is upgrading unit, and this case is extracted and is enriched with while being carried out, and is obtained
Highly concentrated total saposins extracting solution so that concentration amount be greatly reduced, and saves traditional handicraft 2 times filterings, the heavy liquid concentration of wine, refrigeration
Energy consumption, significantly reduce energy consumption；
4) yield of effective component is improved:
5) concentration difference is the motive force of medicinal material extract, and effective component is constantly isolated extraction body during the extraction process by this case
System is conducive to the continuous dissolution of effective component to constantly break the concentration balance between medicinal material and solvent, improves and extracts effect
Rate；Furthermore step is more in actual production, and component damages are more, and compared to traditional aqueous extraction-alcohol precipitation technology, of the invention is effective
The yield of ingredient also improves a lot；
6) improve product purity: bubbling character is peculiar for saponin(e substance, therefore the saponin(e purity ratio that foam fraction factor obtains
Traditional aqueous extraction-alcohol precipitation technology is higher by very much；
7) it safety: can reduce even safer without using organic solvents, production processes such as alcohol.
Detailed description of the invention
Fig. 1 is the schematic diagram of the extraction purification device of invention, and solid arrow indicates liquid flow direction, and dotted arrow indicates foam
Flow direction.
Appended drawing reference:
1. extractor；2. 3. foam separator of sparger；4. pump
Specific embodiment
Carry out the advantage that the present invention is further explained below by specific embodiment.But the present invention includes but is not limited to implement
The specific formula and composition of example.
Embodiment 1:
Process flow:
Process flow as shown in Fig. 1.Extractor 1, pump 4 and sparger 2 are connected, and form circulator, blistering dress
Set 2 it is suitable for reading connect an outlet, access in foam separator.Medicinal material mixes in extractor 1 with solvent, later in extractor 1, pump 4
And it recycles and extracts in sparger 2.It extracts simultaneously, sparger 2 is bubbled, and is made foam from spilling suitable for reading, is collected along pipeline
Into foam separator 3, highly concentrated total saposins extracting solution is obtained after foam fraction factor, and the liquid not blistered in sparger 2
Again it flows back to and participates in extracting in extractor 1.
Extraction step:
Ginseng medicine materical crude slice 200g is added in the dynamic circulation extraction element equipped with electric heating cover, 2L purified water, heating is added
To 80 DEG C, extraction time 4h, circulation rate 10L/h, the capacity of sparger 2 is 0.5L/h, foam separator 3
Revolving speed is 800 turns/min, and the liquid after collecting foam fraction factor is concentrated into equivalent extract, dry.
Comparative example 1:
Traditional batch production method: being added ginseng medicine materical crude slice 200g in the dynamic circulation extraction element equipped with electric heating cover,
2L purified water is added, is heated to 80 DEG C, keep temperature and 4h is recycled with the flow of 10L/h.It is cooling, refrigerated overnight.Filtering, concentration
For 2g/ml, alcohol is sink to 70 °, refrigerates 36h.Filtering, is concentrated into equivalent extract, dry.
The present invention is compared with traditional production method, and indices are as shown in table 1 in the process:
Table 1
As shown in Table 1, the present invention program processing step, production cycle and operating time are obviously shortened, and energy consumption is greatly decreased,
The yield and purity of effective component are largely increased；In addition a part of total saposins are still remained in extracting solution, are such as used as next group
The solvent of extraction can further improve the yield of total saposins.
The measurement method of general ginsenoside: vanilla root rot development process, spectrophotometer measurement.
Embodiment 2:(1) with present invention process prepare general ginsenoside: dress is extracted in the dynamic circulation equipped with electric heating cover
Middle addition ginseng medicine materical crude slice 200g is set, the ethanol solution of 2L25% is added, is heated to 90 DEG C, extraction time 3h, circulation rate is
5L/h, the capacity of sparger 2 are 2.5L/h, and the revolving speed of foam separator 3 is 1400 turns/min, after collecting foam fraction factor
Liquid, be concentrated into equivalent extract, it is dry.
(2) ginseng medicine materical crude slice traditional batch production method: is added in the dynamic circulation extraction element equipped with electric heating cover
2L purified water is added in 200g, is heated to 90 DEG C, keeps temperature and recycles 3h with the flow of 5L/h.It is cooling, refrigerated overnight.Filtering,
Concentration is 2g/ml, and alcohol is sink to 70 °, refrigerates 36h.Filtering, is concentrated into equivalent extract, dry.
The present invention is compared with traditional production method, and indices are as shown in table 2 in the process:
Table 2
Embodiment 3:
(1) general ginsenoside is prepared with present invention process: being added in the dynamic circulation extraction element equipped with electric heating cover
Ginseng medicine materical crude slice 200g, is added the ethanol solution of 2L50%, is heated to 100 DEG C, extraction time 2h, circulation rate 1L/h, blistering
The capacity of device 2 is 5L/h, and the revolving speed of foam separator 3 is 2000 turns/min, the liquid after collecting foam fraction factor, concentration
It is dry to equivalent extract.
(2) ginseng medicine materical crude slice traditional batch production method: is added in the dynamic circulation extraction element equipped with electric heating cover
2L purified water is added in 200g, is heated to 100 DEG C, keeps temperature and recycles 2h with the flow of 1L/h.It is cooling, refrigerated overnight.It crosses
Filter is concentrated as 2g/ml, and alcohol is sink to 70 °, refrigerates 36h.Filtering, is concentrated into equivalent extract, dry.
The present invention is compared with traditional production method, and indices are as shown in table 3 in the process:
Table 3
It should be understood that wt% of the present invention refers to mass percentage.
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (4)
1. a kind of preparation method of saponin(e, it is characterised in that: including following preparation step: (1) medicinal material being placed in extractor, so
After solvent is added, medicinal material mixes in extractor with solvent, later in the extractor, pump and sparger recycle extract,
The extractor is connected with the pump, the sparger, forms circulator；(2) while extracting, sparger is carried out
It is bubbled, the foam of generation is then drawn into extraction system, the liquid not blistered in sparger is flowed back to again in the extractor
It participates in extracting；(3) foam is introduced on the turntable of a foam separator, forms the high dope of saponin(e after turntable is centrifuged
Body；
The saponin(e is ginsenoside.
2. preparation method as described in claim 1, it is characterised in that: the medicinal material is root, stem, leaf and/or flower.
3. preparation method as described in claim 1, it is characterised in that: the solvent is the ethanol solution of water or 30-70wt%,
80~100 DEG C of Extracting temperature, extraction time be 2~4h, volume be 2.5L extractor in, liquid circulation velocity be 1~
10L/h, the revolving speed of Froth centrifugation are not less than 800 turns/min, and the capacity of bubbler is 0.5~5L/min.
4. preparation method as claimed in claim 3, it is characterised in that: the concentration of the ethanol solution is 50wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310062109.3A CN103110678B (en) | 2013-02-27 | 2013-02-27 | A kind of preparation method of saponin(e |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310062109.3A CN103110678B (en) | 2013-02-27 | 2013-02-27 | A kind of preparation method of saponin(e |
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| Publication Number | Publication Date |
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| CN103110678A CN103110678A (en) | 2013-05-22 |
| CN103110678B true CN103110678B (en) | 2019-07-19 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103520030A (en) * | 2013-09-29 | 2014-01-22 | 上海莱博生物科技有限公司 | Preparation method of Chinese herbal compound with natural anti-corrosion effect |
| CN107056705B (en) * | 2017-06-06 | 2023-11-07 | 陕西理工大学 | Energy-saving device and method for separating nuciferine |
| CN111840345A (en) * | 2020-08-25 | 2020-10-30 | 江西纳弗堂制药有限公司 | Extraction process of total saponins of ginseng stem and leaf |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1789220A (en) * | 2005-11-15 | 2006-06-21 | 江西汇仁药业有限公司 | Method for separating Chinese medicinal active substances |
| CN102258883A (en) * | 2011-06-24 | 2011-11-30 | 苏州大学 | Dynamic cycle extraction method for plant extracts and application thereof |
-
2013
- 2013-02-27 CN CN201310062109.3A patent/CN103110678B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1789220A (en) * | 2005-11-15 | 2006-06-21 | 江西汇仁药业有限公司 | Method for separating Chinese medicinal active substances |
| CN102258883A (en) * | 2011-06-24 | 2011-11-30 | 苏州大学 | Dynamic cycle extraction method for plant extracts and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 泡沫分离法分离人参皂苷;修志龙等;《过程工程学报》;20010731;第1卷(第3期);第289页第1-2节 |
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Effective date of registration: 20141219 Address after: 528400 private science and Technology Park, Dongming North Road, Shiqi District, Guangdong, Zhongshan Applicant after: Perfect (China) Co., Ltd. Address before: 200233, building 1, building 333, No. 8, Guiping Road, Shanghai, Xuhui District Applicant before: Shanghai Laibo Bio-chemical Co., Ltd. |
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Effective date of registration: 20200423 Address after: 528400 8 perfect road, Southern China modern Chinese medicine city, Nalong Town, Zhongshan, Guangdong. Co-patentee after: YANGZHOU PERFECT COMMODITY Co.,Ltd. Patentee after: PERFECT (GUANGDONG) COMMODITY Co.,Ltd. Co-patentee after: PERFECT (CHINA) Co.,Ltd. Address before: 528400 private science and Technology Park, Dongming North Road, Shiqi District, Guangdong, Zhongshan Patentee before: PERFECT (CHINA) Co.,Ltd. |
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Effective date of registration: 20210111 Address after: 528400 No. 8, Perfect Road, South China Modern Chinese Medicine City, Nanlang Town, Zhongshan City, Guangdong Province Patentee after: PERFECT (GUANGDONG) COMMODITY Co.,Ltd. Patentee after: YANGZHOU PERFECT COMMODITY Co.,Ltd. Patentee after: PERFECT (CHINA) Co.,Ltd. Patentee after: Guangdong perfect life health Technology Research Institute Co.,Ltd. Address before: 528400 No. 8, Perfect Road, South China Modern Chinese Medicine City, Nanlang Town, Zhongshan City, Guangdong Province Patentee before: PERFECT (GUANGDONG) COMMODITY Co.,Ltd. Patentee before: YANGZHOU PERFECT COMMODITY Co.,Ltd. Patentee before: PERFECT (CHINA) Co.,Ltd. |