CN109232680B - Extraction method of rhodiola rosea - Google Patents
Extraction method of rhodiola rosea Download PDFInfo
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- CN109232680B CN109232680B CN201810925521.6A CN201810925521A CN109232680B CN 109232680 B CN109232680 B CN 109232680B CN 201810925521 A CN201810925521 A CN 201810925521A CN 109232680 B CN109232680 B CN 109232680B
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- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/18—Acyclic radicals, substituted by carbocyclic rings
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Abstract
The invention discloses a rhodiola extraction method, which comprises the following steps of 1) cleaning and slicing raw medicinal materials; 2) flash extracting with 20-30 wt% ethanol water solution with pH of 7.5-8.0; 3) performing secondary extraction with ethanol water solution with ethanol content less than 10%; 4) performing vacuum rotary evaporation; 4) and (4) drying in vacuum. The extraction method has high yield, and the effective component salidroside of radix Rhodiolae is not easily damaged.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine preparations, in particular to a rhodiola rosea extraction method.
Background
Xinnaoxin is a compound preparation prepared by taking Tibetan medicine rhodiola rosea as a main raw material and adding extracts of sea buckthorn and medlar as auxiliary materials; has effects in promoting blood circulation, activating qi-flowing, and nourishing yin. Rhodiola rosea is a perennial herb or shrub plant of rhodiola of Crassulaceae, and contains chemical components such as flavonoid, tyrosol, salidroside, sitosterol, organic acid, volatile oil, polysaccharide, fat, protein and the like. Wherein salidroside has anticancer, anoxia resisting, fatigue resisting, antiaging, arrhythmia resisting, and immunity regulating effects.
The structural formula of salidroside is shown as the following formula:
the Chinese name is 2- (4-hydroxyphenyl) ethyl-beta-D-glucoside, and the molecular formula of salidroside contains 5 hydroxyl groups and two ester groups, and can be well absorbed by human body. It is dissolved in polar solvent such as water and ethanol. The conventional extraction method comprises reflux-extracting with 70% ethanol, recovering solvent under reduced pressure, and refluxing with the ethanol with high concentration to destroy other effective components such as polysaccharide in radix Rhodiolae.
The rhodiola rosea glycoside which is an effective component in the rhodiola rosea has certain hygroscopicity, and deterioration is easily caused when the rhodiola rosea glycoside is prepared into the Xinnaoxin pill, so that the retention period of the rhodiola rosea glycoside is influenced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the extraction method of the rhodiola rosea, which has the advantages that the effective components are not easy to damage and the extraction efficiency is high.
The purpose of the invention is realized by adopting the following technical scheme:
a method for extracting rhodiola root comprises the following steps:
1) taking raw medicinal materials of the rhodiola root tuber, washing with deionized water, and cutting into slices;
2) placing the cut radix Rhodiolae in a flash extractor, adding a first extraction reagent 3-5 times the weight of the cut radix Rhodiolae, and performing flash extraction for 2-4 min; the first extraction reagent is 20-30 vt% ethanol water solution, and the pH value of the first extraction reagent is 7.5-8.0;
3) centrifuging, collecting supernatant, adding a second extraction reagent 3-5 times of the weight of the slices into the residue, and performing flash extraction for 2-4 min; centrifuging, and collecting supernatant, wherein the second extraction reagent is deionized water or ethanol water solution with ethanol content less than 10%; washing the slag with ethanol and water successively; combining the supernatant and the washing solution;
4) vacuum rotary evaporating at 70-80 deg.C, recovering solvent, and concentrating to obtain fluid extract with relative density of 1.23-1.27;
5) vacuum drying at 90-110 deg.C to obtain extract powder with water content less than 5.0%.
Further, in the step 1), drying water, and cutting into pieces. The water in the spin-drying process can effectively avoid the influence of impurities and mixed bacteria outside the original medicine on the extraction process.
Further, in step 2), the first extraction reagent contains sodium bicarbonate in an amount to adjust pH. The sodium bicarbonate can react with acid and alkali, exists in the extraction reagent, and is beneficial to protecting the glucoside group of the salidroside, thereby ensuring higher yield.
Further, in the step 2), the first extraction reagent contains 0.1-0.5 wt% of lactose. Lactose exists as a protective reagent of salidroside and also exists as a modification reagent of the salidroside, so that the water absorption of the salidroside can be effectively reduced, and the storage property of the salidroside is improved.
Further, in step 3), the second extraction reagent contains 0.1-0.3 wt% of EDTA. EDTA as a chelating reagent can effectively promote the dissolution and extraction of trace elements in the rhodiola.
Further, in the step 3), ethanol and water at 0-4 ℃ are used as washing reagents in the washing process.
Further, in step 3), the second extraction reagent is derived from the solvent recovered in step 4). The process can effectively save ethanol. Reduce the discharge of three wastes.
Further, in the step 4), vacuum rotary evaporation is carried out, the steam pressure is less than or equal to 0.3MPa, and the vacuum degree is-0.06-0.1 MPa.
Further, in the step 5), the vacuum degree of vacuum drying is-0.096 to-0.099 MPa; vacuum box drying or vacuum belt continuous drying is adopted.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a rhodiola extraction method, which uses a relatively low-concentration and weakly alkaline ethanol aqueous solution as an extraction reagent, can effectively protect the active ingredient salidroside and improve the extraction rate; the extraction method adopts flash extraction type, breaks the wall at high speed, promotes the release of water-soluble effective components and fat-soluble effective components in the rhodiola rosea, and has no need of long-time heating for extraction, instantaneous extraction of the effective components and less loss;
according to the invention, lactose is added, so that the glucose has glucose group similar to that of salidroside for a long time, the dissolution of the glucose can be effectively promoted, and meanwhile, the hygroscopicity of the salidroside can be effectively improved; the EDTA is added to effectively improve the extraction of the beneficial metal elements.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
The invention provides a rhodiola extraction method, which comprises the following steps:
1) taking raw medicinal materials of the rhodiola root tuber, washing with deionized water, and cutting into slices;
2) placing the cut radix Rhodiolae in a flash extractor, adding a first extraction reagent 3-5 times the weight of the cut radix Rhodiolae, and performing flash extraction for 2-4 min; the first extraction reagent is 20-30 vt% ethanol water solution, and the pH value of the first extraction reagent is 7.5-8.0;
3) centrifuging, collecting supernatant, adding a second extraction reagent 3-5 times the weight of the slices into the residue, and performing flash extraction for 2-4 min; centrifuging, and collecting supernatant, wherein the second extraction reagent is deionized water or ethanol water solution with ethanol content less than 10%; washing the slag with ethanol and water successively; combining the supernatant and the washing solution;
4) vacuum rotary evaporating at 70-80 deg.C, recovering solvent, and concentrating to obtain fluid extract with relative density of 1.23-1.27;
5) vacuum drying at 90-110 deg.C to obtain extract powder with water content less than 5.0%.
The invention effectively extracts the water-soluble effective components in the raw medicinal materials of the rhodiola root and relatively less impurities in the extracting solution compared with part of fat solvent-soluble effective components and high-concentration ethanol by utilizing the extracting reagent with lower ethanol content and alkalescent pH value. The pH value is alkalescent, and the ring body of the salidroside can be effectively protected from being damaged. In the secondary flash extraction process, a reagent with lower ethanol concentration than that in the primary flash extraction process is used as an extraction reagent, so that water-soluble effective components in slag can be effectively dissolved out, and impurities and the like are prevented from being dissolved out; vacuum rotary evaporation at 70-80 deg.C for recovering most of water and organic solvent, and extracting in next batch to obtain fluid extract; drying intermittently or continuously in the air to obtain extract powder, and making into XINNAOXIN pill with other formulas.
Example 1:
a method for extracting rhodiola root comprises the following steps:
1) 1kg of raw medicinal materials of the rhodiola root tuber are taken, washed by deionized water and cut into slices;
2) placing the cut radix Rhodiolae in a flash extractor, adding 4L of the first extraction reagent, and performing flash extraction for 3 min; the first extraction reagent is a 25 vt% ethanol water solution, and the pH value of the first extraction reagent is adjusted to 7.5-8.0 by adding sodium bicarbonate;
3) centrifuging, collecting supernatant, adding 4L of second extraction reagent into residue, and performing flash extraction for 3 min; centrifuging, and taking supernatant, wherein the second extraction reagent is deionized water; washing the slag with 0-4 deg.C ethanol and 0-4 deg.C water successively; combining the supernatant and the washing solution;
4) vacuum rotary evaporating at 75 deg.C under steam pressure of 0.3MPa or less and vacuum degree of-0.06-0.1 MPa, recovering solvent, and concentrating to obtain fluid extract with density of 1.25;
5) drying in a vacuum drying oven at 105 deg.C until the water content is less than 5.0% to obtain 283.1g extract powder.
Example 2:
a method for extracting rhodiola root comprises the following steps:
1) taking 1kg of raw medicinal materials of the rhodiola root tuber, washing with deionized water, and cutting into slices;
2) placing the cut radix Rhodiolae in a flash extractor, adding 4L of the first extraction reagent, and performing flash extraction for 3 min; the first extraction reagent is 20 vt% ethanol water solution, and the pH value of the first extraction reagent is adjusted to 7.5-8.0 by adding sodium bicarbonate; the first extraction reagent contains 0.5 wt% lactose;
3) centrifuging, collecting supernatant, adding 4L of second extraction reagent into residue, and performing flash extraction for 3 min; centrifuging, and taking supernatant, wherein the second extraction reagent is deionized water; washing the slag body with 0-4 ℃ ethanol and 0-4 ℃ water in sequence; combining the supernatant and the washing solution;
4) vacuum rotary evaporating at 75 deg.C under steam pressure of 0.3MPa or less and vacuum degree of-0.06-0.1 MPa, recovering solvent, and concentrating to obtain fluid extract with density of 1.25;
5) drying in a vacuum drying oven at 105 deg.C, and vacuum drying to obtain extract powder with water content less than 5.0% to obtain 292.6g extract powder.
Example 3:
a method for extracting radix Rhodiolae comprises the following steps:
1) taking 1kg of raw medicinal materials of the rhodiola root tuber, washing with deionized water, and cutting into slices;
2) placing the cut radix Rhodiolae in a flash extractor, adding 4L of the first extraction reagent, and performing flash extraction for 3 min; the first extraction reagent is 30 vt% ethanol water solution, and the pH value of the first extraction reagent is adjusted to 7.5-8.0 by adding sodium bicarbonate; the first extraction reagent contains 0.5 wt% lactose;
3) centrifuging, collecting supernatant, adding 4L second extraction reagent into the residue, and flash extracting for 3 min; centrifuging, and collecting supernatant, wherein the second extraction reagent is 5 wt% ethanol water solution, and the second extraction solvent contains 0.2 wt% EDTA; washing the slag body with 0-4 ℃ ethanol and 0-4 ℃ water in sequence; combining the supernatant and the washing solution;
4) vacuum rotary evaporating at 75 deg.C under steam pressure of 0.3MPa or less and vacuum degree of-0.06-0.1 MPa, recovering solvent, and concentrating to obtain fluid extract with density of 1.25;
5) drying in a vacuum drying oven at 105 deg.C until the water content is less than 5.0%, to obtain 289.3g extract powder.
Comparative example 1:
a method for extracting rhodiola root comprises the following steps:
1) taking 1kg of raw medicinal materials of the rhodiola root tuber, washing with deionized water, and cutting into slices;
2) placing the cut radix Rhodiolae in a flash extractor, adding 4L of the first extraction reagent, and performing flash extraction for 3 min; the first extraction reagent is a 30 vt% ethanol aqueous solution;
3) centrifuging, collecting supernatant, adding 4L of second extraction reagent into residue, and performing flash extraction for 3 min; centrifuging, and taking supernatant, wherein the second extraction reagent is 5 wt% ethanol water solution; washing the slag with ethanol and water successively; combining the supernatant and the washing solution;
4) vacuum rotary evaporating at 75 deg.C under steam pressure of 0.3MPa or less and vacuum degree of-0.06-0.1 MPa, recovering solvent, and concentrating to obtain fluid extract with density of 1.25;
5) drying in a vacuum drying oven at 105 deg.C, and vacuum drying to obtain extract powder with water content less than 5.0% to obtain 266.5g extract powder.
Comparative example 2:
a method for extracting rhodiola root comprises the following steps:
1) taking 1kg of raw medicinal materials of the rhodiola root tuber, washing with deionized water, and cutting into slices;
2) placing the cut radix Rhodiolae in a flash extractor, adding 4L of the first extraction reagent, and performing flash extraction for 3 min; the first extraction reagent is deionized water;
3) centrifuging, collecting supernatant, adding 4L of second extraction reagent into residue, and performing flash extraction for 3 min; centrifuging, and taking supernatant, wherein the second extraction reagent is deionized water; washing the slag body with water; combining the supernatant and the washing solution;
4) vacuum rotary evaporating at 75 deg.C under steam pressure of 0.3MPa or less and vacuum degree of-0.06-0.1 MPa, recovering solvent, and concentrating to obtain fluid extract with density of 1.25;
5) drying in a vacuum drying oven at 105 deg.C until the water content is less than 5.0% to obtain 226.9g extract powder.
Comparative example 3:
a method for extracting rhodiola root comprises the following steps:
1) taking 1kg of raw medicinal materials of the rhodiola root tuber, washing with deionized water, and cutting into slices;
2) placing the cut radix Rhodiolae in a flash extractor, adding 4L deionized water, and decocting at 95-100 deg.C for 48 hr;
3) centrifuging, collecting supernatant, adding 4L deionized water into the residue, and decocting at 95-100 deg.C for 48 hr; centrifuging and taking supernatant; washing the slag body with water; combining the supernatant and the washing solution;
4) vacuum rotary evaporating at 75 deg.C under steam pressure of 0.3MPa or less and vacuum degree of-0.06-0.1 MPa, recovering solvent, and concentrating to obtain fluid extract with density of 1.25;
5) drying in a vacuum drying oven at 105 deg.C until the water content is less than 5.0%, to obtain 244.6g extract powder.
Performance detection and Effect evaluation
Dissolving the extract powder obtained in the examples 1-3 and the comparative examples 1-3, taking the powder with unit weight, fixing the volume, detecting the content of the salidroside by using high performance liquid chromatography, and calculating the extraction rate of the salidroside:
wherein p is the extraction rate;
m1g, the amount of the obtained extract powder;
v is the volume of the monomer weight powder diluent with constant volume, mL/g;
m2weight of raw medicine, g;
C1the concentration of the diluent is mg/mL;
the results are shown in the following table:
TABLE 1 extraction rate of salidroside
| Example 1 | Example 2 | Example 3 |
| 2.96％ | 3.31％ | 3.40％ |
| Comparative example 1 | Comparative example 2 | Comparative example 3 |
| 2.53％ | 2.45％ | 2.28％ |
From the above table, the method provided by the invention can effectively improve the yield of salidroside in rhodiola rosea, and compared with the traditional water boiling extraction process, the yield is as high as 50%. Has better market application prospect.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (7)
1. The extraction method of the rhodiola is characterized by comprising the following steps:
1) taking raw medicinal materials of the rhodiola root tuber, washing with deionized water, and cutting into slices;
2) placing the cut radix Rhodiolae in a flash extractor, adding a first extraction reagent 3-5 times the weight of the cut radix Rhodiolae, and performing flash extraction for 2-4 min; the first extraction reagent is 20-30 vt% ethanol water solution, and the pH value of the first extraction reagent is 7.5-8.0; the first extraction reagent contains 0.1-0.5 wt% lactose;
3) centrifuging, collecting supernatant, adding a second extraction reagent 3-5 times the weight of the slices into the residue, and performing flash extraction for 2-4 min; centrifuging, and collecting supernatant, wherein the second extraction reagent is deionized water or ethanol water solution with ethanol content less than 10%, and contains 0.1-0.3 wt% of EDTA; washing the slag with ethanol and water successively; combining the supernatant and the washing solution;
4) vacuum rotary evaporating at 70-80 deg.C, recovering solvent, and concentrating to obtain fluid extract with relative density of 1.23-1.27;
5) vacuum drying at 90-110 deg.C to obtain extract powder with water content less than 5.0%.
2. The extraction method according to claim 1, wherein in step 1), the water is dried and cut into pieces.
3. The extraction method according to claim 1, wherein in the step 2), the first extraction reagent contains a pH-adjusting amount of sodium bicarbonate.
4. The extraction method according to claim 1, wherein in the step 3), ethanol and water at 0-4 ℃ are used as washing reagents in the washing process.
5. The extraction process of claim 1, wherein in step 3) the second extraction reagent is derived from the solvent recovered in step 4).
6. The extraction method as claimed in claim 1, wherein in step 4), vacuum rotary evaporation is carried out, the steam pressure is less than or equal to 0.3MPa, and the vacuum degree is-0.06 to-0.1 MPa.
7. The extraction method according to claim 1, wherein in the step 5), the vacuum degree of vacuum drying is-0.096 to-0.099 MPa; vacuum box drying or vacuum belt continuous drying is adopted.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104306427A (en) * | 2014-11-06 | 2015-01-28 | 广州神农生物技术有限公司 | Rhodiola rosea extract and application thereof |
| CN106413687A (en) * | 2015-09-01 | 2017-02-15 | 拉芳家化股份有限公司 | Product containing Rhodiola extract and Ginkgo biloba extract, and preparation method and use thereof |
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| TWI398447B (en) * | 2010-07-20 | 2013-06-11 | Taipei Medical University Tmu | Compounds and method for inhibiting the activity of gelatinase and collagenase |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104306427A (en) * | 2014-11-06 | 2015-01-28 | 广州神农生物技术有限公司 | Rhodiola rosea extract and application thereof |
| CN106413687A (en) * | 2015-09-01 | 2017-02-15 | 拉芳家化股份有限公司 | Product containing Rhodiola extract and Ginkgo biloba extract, and preparation method and use thereof |
Non-Patent Citations (3)
| Title |
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| "乳糖研磨改性降低红景天提取物吸湿性的工艺与原理研究";张定堃 等;《中国中药杂志》;20140430;第39卷(第8期);第1413-1420页 * |
| "闪式提取红景天苷工艺优化研究";范桂强 等;《中国药师》;20161231;第19卷(第1期);第40-42页 * |
| 范桂强 等."闪式提取红景天苷工艺优化研究".《中国药师》.2016,第19卷(第1期),第40-42页. * |
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