CN103110678A - Method for preparing saponin - Google Patents
Method for preparing saponin Download PDFInfo
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- CN103110678A CN103110678A CN2013100621093A CN201310062109A CN103110678A CN 103110678 A CN103110678 A CN 103110678A CN 2013100621093 A CN2013100621093 A CN 2013100621093A CN 201310062109 A CN201310062109 A CN 201310062109A CN 103110678 A CN103110678 A CN 103110678A
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- Prior art keywords
- saponin
- extraction
- preparation
- concentration
- foam
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229930182490 saponin Natural products 0.000 title claims abstract description 31
- 150000007949 saponins Chemical class 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 20
- 238000000605 extraction Methods 0.000 claims abstract description 40
- 239000006260 foam Substances 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 230000005587 bubbling Effects 0.000 claims abstract description 7
- 229930182494 ginsenoside Natural products 0.000 claims abstract description 7
- 229940089161 ginsenoside Drugs 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 239000000284 extract Substances 0.000 claims description 10
- 239000012567 medical material Substances 0.000 claims description 8
- 230000001476 alcoholic effect Effects 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 16
- 241000208340 Araliaceae Species 0.000 abstract description 12
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 abstract description 12
- 235000003140 Panax quinquefolius Nutrition 0.000 abstract description 12
- 235000008434 ginseng Nutrition 0.000 abstract description 12
- 238000001035 drying Methods 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 8
- 238000012546 transfer Methods 0.000 abstract description 2
- 239000004480 active ingredient Substances 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 238000004904 shortening Methods 0.000 abstract 1
- 235000017709 saponins Nutrition 0.000 description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 15
- 239000004615 ingredient Substances 0.000 description 8
- 238000004321 preservation Methods 0.000 description 8
- 238000005265 energy consumption Methods 0.000 description 7
- 238000005485 electric heating Methods 0.000 description 6
- 101100298222 Caenorhabditis elegans pot-1 gene Proteins 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000008213 purified water Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003809 water extraction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000419 plant extract Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Substances OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Steroid Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for preparing saponin. The method comprises the following steps of: (1) adding roots, stems, leaves or flowers of ginseng into an extracting tank and adding a solvent to perform dynamic outer circulation extraction; (2) bubbling on an extraction loop by using a bubbling device, and discharging and collecting foams; (3) breaking and removing the collected foams by using a foam separating device to obtain high-concentration total saponin liquid; and (4) performing conventional concentration and drying treatment on the high-concentration total saponin liquid. By adopting the method for preparing the saponin, based on the characteristic that ginsenoside is likely to generate bubbles, the disadvantages of a conventional process is changed into advantages, and the problems of low transfer rate of active ingredients, more steps, difficulty in concentration, long operation cycle, high cost and the like of an existing preparation process are solved. By fully using the characteristics of the dynamic outer circulation extraction and possibility of bubble generation of the saponin, a reasonable design is carried out, and separation during extraction can be performed to obtain the high-concentration total saponin liquid, so that the aims of simplifying process steps, shortening the production cycle and improving the yield and the like are achieved.
Description
Technical field
The present invention relates to a kind of preparation method of saponin.
Background technology
At present to prepare the most frequently used method is water extraction, concentrated, precipitate with ethanol, concentrated, drying process to Radix Ginseng total saponins, the concentration operation difficulty of this method water extraction liquid is large, whole processing step is loaded down with trivial details, production cycle is long, and the equipment that needs is many, and energy consumption is large, the loss of effective ingredient is large, purity is low, and production cost is higher, and uses in a large number both dangerous also not environmental protection of ethanol.
Water extraction, resin separation purification, concentrated, drying process are also arranged, and this technological advantage is that ginsenoside's purity is higher, but shortcoming is to use in a large number resin and ethanol, and cost is very high, and is higher to workman's operation requirements, and safety and environmental protection are relatively poor.
The contradiction of plant extract industry development and pollution, the contradiction of high investment and low output is compeled to be solved, utilizing substance characteristics to carry out reasonably optimizing, combination in conjunction with the operating feature of existing device, is the feasible thinking of the problems such as energy-conservation, high-quality, environmental protection and sustainable development that solve the plant extract industry development.
Summary of the invention
it is many that technical problem to be solved by this invention is to have overcome traditional step of preparation process, concentrated difficulty, production cycle is long, the effective ingredient rate of transform is low, energy consumption is large, the technical problems such as a large amount of uses of ethanol, characteristic of bubbling easy of the ginsenoside, transfer this shortcoming that it has been generally acknowledged that to advantage, dynamic outer circulating extracting and Bubble fractionation are combined, reduce concentrated, the steps such as wine is heavy, reach the simplification processing step, shorten the production cycle, reduce energy consumption, improve the effective ingredient yield, avoid using the effect of the organic solvents such as ethanol, simplifying the operation, energy-conserving and environment-protective, production safety, save on cost significant contribution is arranged.
The invention provides a kind of preparation method of saponin, comprise following concrete steps:
(1) medical material is placed in extraction pot, add entry, or lower than 50 alcoholic solution of spending, carry out dynamic outer circulating extracting in 80 ~ 100 ℃, for volume 2.5L extraction pot, its circulation rate is 1 ~ 10L/h, and the extraction pot of other volumes changes uninterrupted with the principle that linear velocity equates, extraction time is 2 ~ 4h;
(2) extraction simultaneously or afterwards, sparger carries out bubbling, and capacity is 0.5 ~ 5L/min, pressing the volume ratio of sparger amplifies, foam is overflowed from suitable for reading, collect along pipeline and enter foam separator, and the liquid that does not bubble in sparger flows back to participation extraction in extraction pot again.
(3) the foam separator rotating speed for turning/min greater than 800, obtains high dense total saponins extracting solution after foam separation.
In the present invention, described medical material is root, stem, leaf and/or flower.
In the present invention, described saponin is high saponin content medical material.Preferably, described saponin is the ginsenoside.
In the present invention, the method of described extraction solvent is for putting water the alcoholic solution to 30-70wt%, extract 80 ~ 100 ℃ of temperature, extraction time is 2 ~ 4h, be in the extraction pot of 2.5L at volume, liquid circulation velocity is 1 ~ 10L/h, and the centrifugal rotating speed of Froth turns/min for being not less than 800, and the capacity of bubbler is 0.5 ~ 5L/min.Preferably, the concentration of described alcoholic solution is 50wt%.
Technique effect of the present invention is:
1) the present invention is the characteristic that takes full advantage of saponin, as long as existing equipment is done less change, can realize the method, and ginsenoside's preparation cost is significantly reduced, and Environmental Safety more;
2) simplify processing step, shorten the production cycle: this technique leaching process and ginsenoside's enrichment process carry out simultaneously, make high dense Radix Ginseng total saponins liquid, have significantly reduced concentrated amount, and have saved the steps such as traditional filtration, wine are heavy, cold preservation;
3) energy efficient: the operating unit of energy consumption maximum is upgrading unit, and this case extraction and enrichment are carried out simultaneously, obtain high dense total saponins extracting solution, thereby have significantly reduced concentrated amount, and save that traditional handicraft 2 times is filtered, the heavy liquid of wine is concentrated, the energy consumption of cold preservation, greatly reduced energy consumption;
4) improve the yield of effective ingredient:
5) concentration difference is the motive force of medicinal material extract, and the extraction system is constantly isolated effective ingredient in this case in leaching process, thereby constantly breaks the concentration balance between medical material and solvent, is conducive to the continuous stripping of effective ingredient, improves extraction efficiency; In actual production, step is more in addition, and the composition loss is more, and than traditional aqueous extraction-alcohol precipitation technology, the yield of effective ingredient of the present invention also improves a lot;
6) improve product purity: bubbling character is that the saponins material is peculiar, so the saponin purity that foam separation obtains exceeds much than traditional aqueous extraction-alcohol precipitation technology;
7) safety: can reduce organic solvents such as even not using ethanol, production process is safer.
Description of drawings
Fig. 1 flows to for the schematic diagram of extraction purification devices of invention, solid arrow express liquid, dotted arrow represent foam stream to.
Reference numeral:
1. extraction pot; 2. sparger 3. foam separators; 4. pump
The specific embodiment
Further set forth advantage of the present invention below by the specific embodiment.But the present invention includes but be not limited to concrete formula and the composition of embodiment.
Embodiment 1:
Technological process:
Technological process as shown in Figure 1.Extraction pot 1, pump 4 and sparger 2 are connected, and form circulating device, and sparger 2 is suitable for reading connects an outlet, in the access foam separator.Medical material in extraction pot 1 with solvent, circulation is extracted in extraction pot 1, pump 4 and sparger 2 afterwards.The extraction while, sparger 2 carries out bubbling, and foam is overflowed from suitable for reading, collects along pipeline and enters foam separator 3, obtain high dense total saponins extracting solution after foam separation, and the liquid that does not bubble in sparger 2 flows back to participation extraction in extraction pot 1 again.
Extraction step:
In being housed, the dynamic circulation extraction element of electric heating cover adds Radix Ginseng decoction pieces 200g, add the 2L purified water, be heated to 80 ℃, extraction time is 4h, and circulation rate is 10L/h, and the capacity of sparger 2 is 0.5L/h, the rotating speed of foam separator 3 is 800 to turn/min, liquid after the collection foam separation is concentrated into equivalent extract, drying.
The comparative example 1:
The traditional batch mode of production: add Radix Ginseng decoction pieces 200g in the dynamic circulation extraction element of electric heating cover is housed, adds the 2L purified water, be heated to 80 ℃, keep temperature and with the flow circulation 4h of 10L/h.Cooling, cold preservation is spent the night.Filter, simmer down to 2g/ml, alcohol are sink to 70 °, cold preservation 36h.Filter, be concentrated into equivalent extract, drying.
The present invention compares with traditional mode of production, and in process, indices is as shown in table 1:
Table 1
As shown in Table 1, the present invention program's processing step, production cycle and operating time obviously shorten, and energy consumption significantly reduces, and yield and the purity of effective ingredient are largely increased; Residual a part of total saponins still in extracting solution, as the solvent that extracts as next group, can further improve the yield of total saponins in addition.
The measuring method of Radix Ginseng total saponins: vanillin-perchloric acid development process, spectrophotometer measurement.
Embodiment 2:(1) prepare Radix Ginseng total saponins with technique of the present invention: add Radix Ginseng decoction pieces 200g in the dynamic circulation extraction element of electric heating cover is housed, the alcoholic solution that adds 2L25%, be heated to 90 ℃, extraction time is 3h, and circulation rate is 5L/h, and the capacity of sparger 2 is 2.5L/h, the rotating speed of foam separator 3 is 1400 to turn/min, liquid after the collection foam separation is concentrated into equivalent extract, drying.
(2) the traditional batch mode of production: add Radix Ginseng decoction pieces 200g in the dynamic circulation extraction element of electric heating cover is housed, adds the 2L purified water, be heated to 90 ℃, keep temperature and with the flow circulation 3h of 5L/h.Cooling, cold preservation is spent the night.Filter, simmer down to 2g/ml, alcohol are sink to 70 °, cold preservation 36h.Filter, be concentrated into equivalent extract, drying.
The present invention compares with traditional mode of production, and in process, indices is as shown in table 2:
Table 2
Embodiment 3:
(1) prepare Radix Ginseng total saponins with technique of the present invention: add Radix Ginseng decoction pieces 200g in the dynamic circulation extraction element of electric heating cover is housed, the alcoholic solution that adds 2L50%, be heated to 100 ℃, extraction time is 2h, and circulation rate is 1L/h, and the capacity of sparger 2 is 5L/h, the rotating speed of foam separator 3 is 2000 to turn/min, liquid after the collection foam separation is concentrated into equivalent extract, drying.
(2) the traditional batch mode of production: add Radix Ginseng decoction pieces 200g in the dynamic circulation extraction element of electric heating cover is housed, adds the 2L purified water, be heated to 100 ℃, keep temperature and with the flow circulation 2h of 1L/h.Cooling, cold preservation is spent the night.Filter, simmer down to 2g/ml, alcohol are sink to 70 °, cold preservation 36h.Filter, be concentrated into equivalent extract, drying.
The present invention compares with traditional mode of production, and in process, indices is as shown in table 3:
Table 3
Should be understood that, wt% of the present invention all refers to the quality percentage composition.
Above specific embodiments of the invention are described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, not breaking away from impartial conversion and the modification of doing under the spirit and scope of the present invention, all should contain within the scope of the invention.
Claims (6)
1. the preparation method of a saponin is characterized in that: comprise following preparation process:
(1) medical material is placed in extraction pot, then adds solvent to carry out dynamic outer circulating extracting;
When (2) extracting or carry out bubbling on closed circuit outside afterwards, then the foam that produces is drawn the extraction system;
(3) described foam is introduced on the rotating disk of a foam separator, formed the high dope body of saponin after rotating disk is centrifugal.
2. preparation method as claimed in claim 1, it is characterized in that: described medical material is root, stem, leaf and/or flower.
3. preparation method as claimed in claim 1, it is characterized in that: described saponin is high saponin content medical material.
4. preparation method as claimed in claim 3 is characterized in that: described saponin is the ginsenoside.
5. preparation method as claimed in claim 1, it is characterized in that: the method for described extraction solvent is for putting water the alcoholic solution to 30-70wt%, extract 80 ~ 100 ℃ of temperature, extraction time is 2 ~ 4h, be in the extraction pot of 2.5L at volume, liquid circulation velocity is 1 ~ 10L/h, and the centrifugal rotating speed of Froth turns/min for being not less than 800, and the capacity of bubbler is 0.5 ~ 5L/min.
6. preparation method as claimed in claim 5, it is characterized in that: the concentration of described alcoholic 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 |
|---|---|
| CN103110678A true CN103110678A (en) | 2013-05-22 |
| CN103110678B CN103110678B (en) | 2019-07-19 |
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Cited By (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 |
| CN107056705A (en) * | 2017-06-06 | 2017-08-18 | 陕西理工大学 | A kind of apparatus and method of energy-saving separation 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 |
|---|
| 修志龙等: "泡沫分离法分离人参皂苷", 《过程工程学报》 * |
Cited By (4)
| 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 |
| CN107056705A (en) * | 2017-06-06 | 2017-08-18 | 陕西理工大学 | A kind of apparatus and method of energy-saving separation Nuciferine |
| 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 |
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| Publication number | Publication date |
|---|---|
| CN103110678B (en) | 2019-07-19 |
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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. |