CN1786011A - Method of preparing Rhodiola sacra glycoside - Google Patents
Method of preparing Rhodiola sacra glycoside Download PDFInfo
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- CN1786011A CN1786011A CN 200510111859 CN200510111859A CN1786011A CN 1786011 A CN1786011 A CN 1786011A CN 200510111859 CN200510111859 CN 200510111859 CN 200510111859 A CN200510111859 A CN 200510111859A CN 1786011 A CN1786011 A CN 1786011A
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Abstract
The present invention relates to a method for preparing rhodiola glucoside crude product by using glassy privet fruit as raw material and adopting macroporous adsorption resin purification technique. Said method includes the following steps: using 60%-80% ethyl alcohol to soak broken glossy privet fruit to obtain rhodiola glucoside extract, then making the obtained rhodiola glucoside extract undergo the processes of low-polar AB-8 type macroporous resin adsorption, washing with pure clean water, 25-35% ethyl alcohol elution, recovering ethyl alcohol and concentration so as to obtain the rhodiola glucoside crude product.
Description
Technical field
The present invention relates to medical technical field, is a kind of preparation method who extracts rhodioside from Glossy Privet Fruit.
Background technology
Rhodioside; English name salidroside; chemical name " to the oxybenzene ethyl-(p-hydroxyphenethyl-β-D-glucoside) "; systematic naming method: 1-(4-hydroxyl) styroyl-β-D-glucopyranoside; it is a kind of active compound that obtains that from medicinal plant, extracts; rhodioside have strengthen learning and memory, improve cardio-cerebrovascular, the effect of antifatigue, hypoxia tolerance, anti-ageing, enhancing immunity, antiviral and protection internal organs, be a kind of medicine (Qu Zhiwei of environmental adaptation unit that DEVELOPMENT PROSPECT is arranged very much.The progress of Root of Kirilow Rhodiola, Chinese practical traditional Chinese and western medicine magazine, 2005 the 18th the 7th phases of volume: 1063-1065).At present, if the drug main that utilizes the exploitation of this compound with natural Rhodida plant as raw material.But the Root of Kirilow Rhodiola major part is born in height above sea level 3500 to limestone, grouan, water river, mountain region or the mountain valley rock of 5000m.Obtain difficulty, cost an arm and a leg, and because Root of Kirilow Rhodiola in the exploitation of industrial aspect such as medicine, food, has consumed a large amount of natural plant resources, and wild plant is excavated in a large number, resource is exhausted day by day, and (Zhao Yong calls out, Liu Chenghai, Wu Tinghua.The research of Root of Kirilow Rhodiola and progress, the secondary special product of Chinese woods, 1998 the 3rd phases: 44-45).In order to protect this rare species, attempt in recent years Rhodida plant is carried out artificial culture, still; rhodioside content under the artificial cultivation condition low (being lower than 0.2%); the seedling root rot is serious, and need take the big area arable land, limits the popularization of this technology.Obtain effect preferably though cell large scale is cultivated, cultivated the cost height, be difficult for carrying out scale operation.(Xu Jianfeng, Ying Peiqing, Su Zhiguo.Radix Rhodiolae resource applicating and exploitation progress.Herbal medicine, 1998 the 29th the 3rd phases of volume: 202-205)
Summary of the invention
The invention provides a kind of is the method for feedstock production rhodioside with the Chinese medicine Glossy Privet Fruit.Glossy Privet Fruit is the dry fruit of Oleaceae plant glossy privet (Ligustrum lucidum Ait.), the Shennong's Herbal row be top grade, " bitter is flat, main bowl spares, five viscera settling is supported spirit, removes sick." have a function of nourishing liver and kidney, strong waist knee, improve visual and auditory acuity; cure mainly the hepatic and renal YIN deficiency, have a dizzy spell, (Li Baohua, the research situation of Glossy Privet Fruit, Chinese medical research and practice; in July, 2004, the 2nd the 7th phases of volume: 49-51) such as tinnitus, hair color, soreness of the waist and knees.The development research of Glossy Privet Fruit has very early in China to be carried out, and has just begun to use Glossy Privet Fruit in ancient times as setting upright medicine.The modern pharmacology experiment shows that Glossy Privet Fruit has hepatic cholagogic, antisepsis and anti-inflammation, antitumor, various pharmacological activities such as reducing blood-fat is hypoglycemic, strengthening immunity.Glossy Privet Fruit belongs to resourceful secondary product of forestry in China, and it is very extensive to distribute, and areas such as East China, south China, southwest, Central China all have.In the mountain area, all there is plantation in Plain, flower garden.Except wild, tame in addition.Glossy Privet Fruit is an evergreen plant, can beautify the environment again, and particularly the annual maturation of Glossy Privet Fruit once year can be gathered in the crops every year, and aboundresources can guarantee to large-scale develop and utilize for a long time.
The present invention prepares the method for rhodioside with Glossy Privet Fruit, and step is as follows:
1. the preparation of rhodioside extracting solution: with using the 60-80% alcohol immersion more than 24 hours routinely after the Glossy Privet Fruit pulverizing, reclaim filtrate, extract 2-3 time, merging filtrate gets the rhodioside extracting solution behind the recovery ethanol.
2. the purifying of rhodioside crude product: with said extracted liquid through absorption with macroporous adsorbent resin, with purified rinse water to the Molish reaction negative, 25%-35% ethanol with 2 times of amounts of resin bed volume carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again by the same method through absorption with macroporous adsorbent resin, purified rinse water to Molish reaction negative, 2 times of amount 25%-35% ethanol elutions, elutriant promptly gets the rhodioside crude product through reclaiming ethanol and concentrating after the drying.
Above-mentioned Glossy Privet Fruit is commercially available Chinese medicine Glossy Privet Fruit, and said macroporous adsorbent resin is selected from low-pole AB-8 type macroporous adsorbent resin, nonpolar 1300 type macroporous adsorbent resins.
The present invention compared with prior art has the following advantages:
1. do not have organic residual, safe: in the whole processing method except adding ethanol, need not additional organic solvents, ethanol is easy to reclaim, do not have organic residual, the security of products height.
2. method is simple, and is easy and simple to handle: this preparation method carries out at normal temperatures and pressures, and the method simple operations is convenient, is fit to the needs of industrialized production.
3. raw material sources are wide, easily obtain, and low price, cost is low, and the rhodioside extraction yield is not less than 0.3% (wt), and the content of rhodioside is not less than 6% in the rhodioside crude product.
Embodiment
Now in conjunction with the embodiments, the present invention is explained in detail.
Embodiment 1: after the 1kg Glossy Privet Fruit is pulverized, adds 3kg80% ethanol, stirs and thorough mixing, soaked 48 hours, reclaim filtrate, extract three times, and merging filtrate, reduced-pressure backflow reclaims ethanol and gets the rhodioside extracting solution; With extracting solution through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, with purified rinse water to the Molish reaction negative, ethanol with 2 times of amounts 30% carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, to the flushing of Molish reaction negative, carry out wash-out with the ethanol of 2 times of amounts 30% with purified rinse water, elutriant gets rhodioside crude product 3.065g through reclaiming ethanol and concentrating after the vacuum-drying.Prepared rhodioside crude product is further purified under following chromatographic condition through polyamide column and detects: Hypersil-C
18The analysis chromatographic column (5 μ m, 4.6mm * 150mm); Moving phase: methanol-water (20: 80); Flow velocity: 0.4ml/min; Detect wavelength: 220nm; Sample size 20 μ l; Sensitivity: 0.010AUFS.The result shows that the rhodioside crude product of preparation has identical chromatographic peak with the rhodioside standard substance at 12min, is confirmed that it is rhodioside, and rhodioside content is 6.32% in the rhodioside crude product.
Embodiment 2: after the 1kg Glossy Privet Fruit is pulverized, adds 3kg70% ethanol, stirs and thorough mixing, soaked 72 hours, reclaim filtrate, extract secondary, and merging filtrate, reduced-pressure backflow reclaims ethanol and gets the rhodioside extracting solution; With extracting solution through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, with purified rinse water to the Molish reaction negative, ethanol with 2 times of amounts 35% carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, to the Molish reaction negative, carry out wash-out with the ethanol of 2 times of amounts 35% with purified rinse water, elutriant gets rhodioside crude product 2.988g through reclaiming ethanol and concentrating after the vacuum-drying.Prepared rhodioside crude product after polyamide column is further purified, with embodiment 1 described high performance liquid chromatography detect in the rhodioside crude product content of rhodioside be 6.03%.
Embodiment 3: after the 1kg Glossy Privet Fruit is pulverized, adds 4kg60% ethanol, stirs and thorough mixing, soaked 72 hours, reclaim filtrate, extract three times, and merging filtrate, reduced-pressure backflow reclaims ethanol and gets the rhodioside extracting solution; With extracting solution through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, with purified rinse water to the Molish reaction negative, ethanol with 2 times of amounts 35% carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, to the Molish reaction negative, carry out wash-out with the ethanol of 2 times of amounts 35% with purified rinse water, elutriant is rhodioside crude product 3.012g after the vacuum-drying through reclaiming ethanol and concentrating.Prepared rhodioside crude product after polyamide column is further purified, with embodiment 1 described high performance liquid chromatography detect in the rhodioside crude product content of rhodioside be 7.21%.
Embodiment 4: after the 1kg Glossy Privet Fruit is pulverized, adds 4kg70% ethanol, stirs and thorough mixing, soaked 48 hours, reclaim filtrate, extract secondary, and merging filtrate, reduced-pressure backflow reclaims ethanol and gets the rhodioside extracting solution; With extracting solution through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, with purified rinse water to the Molish reaction negative, ethanol with 2 times of amounts 25% carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, to the Molish reaction negative, carry out wash-out with the ethanol of 2 times of amounts 25% with purified rinse water, elutriant gets rhodioside crude product 2.983g through reclaiming ethanol and concentrating after the vacuum-drying.Prepared rhodioside crude product after polyamide column is further purified, with embodiment 1 described high performance liquid chromatography detect in the rhodioside crude product content of rhodioside be 6.98%.
Embodiment 5: after the 1kg Glossy Privet Fruit is pulverized, adds 5kg70% ethanol, stirs and thorough mixing, soaked 48 hours, reclaim filtrate, extract three times, and merging filtrate, reduced-pressure backflow reclaims ethanol and gets the rhodioside extracting solution; With extracting solution through nonpolar 1300 type absorption with macroporous adsorbent resin 30min, with purified rinse water to the Molish reaction negative, ethanol with 2 times of amounts 35% carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again through nonpolar 1300 type absorption with macroporous adsorbent resin 30min, to the Molish reaction negative, carry out wash-out with the ethanol of 2 times of amounts 35% with purified rinse water, elutriant gets rhodioside crude product 2.316g through reclaiming ethanol and concentrating after the vacuum-drying.Prepared rhodioside crude product after polyamide column is further purified, with embodiment 1 described high performance liquid chromatography detect in the rhodioside crude product content of rhodioside be 4.11%.
Embodiment 6: after the 1kg Glossy Privet Fruit is pulverized, adds 4kg70% ethanol, stirs and thorough mixing, soaked 48 hours, reclaim filtrate, extract three times, and merging filtrate, reduced-pressure backflow reclaims ethanol and gets the rhodioside extracting solution; With extracting solution through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, with purified rinse water to the Molish reaction negative, ethanol with 2 times of amounts 30% carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, to the Molish reaction negative, carry out wash-out with the ethanol of 2 times of amounts 30% with purified rinse water, elutriant gets rhodioside crude product 3.3g through reclaiming ethanol and concentrating after the vacuum-drying.Prepared rhodioside crude product after polyamide column is further purified, with embodiment 1 described high performance liquid chromatography detect in the rhodioside crude product content of rhodioside be 7.7%.
Embodiment 7: after the 1kg Glossy Privet Fruit is pulverized, adds 5kg70% ethanol, stirs and thorough mixing, soaked 48 hours, reclaim filtrate, extract three times, and merging filtrate, reduced-pressure backflow reclaims ethanol and gets the rhodioside extracting solution; With extracting solution through nonpolar 1300 type absorption with macroporous adsorbent resin 30min, with purified rinse water to the Molish reaction negative, ethanol with 2 times of amounts 35% carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again through nonpolar 1300 type absorption with macroporous adsorbent resin 30min, to the Molish reaction negative, carry out wash-out with the ethanol of 2 times of amounts 35% with purified rinse water, elutriant gets rhodioside crude product 2.036g through reclaiming ethanol and concentrating after the vacuum-drying.Prepared rhodioside crude product after polyamide column is further purified, with embodiment 1 described high performance liquid chromatography detect in the rhodioside crude product content of rhodioside be 3.15%.
Embodiment 8: after the 1kg Glossy Privet Fruit is pulverized, adds 4kg80% ethanol, stirs and thorough mixing, soaked 24 hours, reclaim filtrate, extract three times, and merging filtrate, reduced-pressure backflow reclaims ethanol and gets the rhodioside extracting solution; With extracting solution through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, with purified rinse water to the Molish reaction negative, ethanol with 2 times of amounts 25% carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, to the Molish reaction negative, carry out wash-out with the ethanol of 22 times of amounts 5% with purified rinse water, elutriant gets rhodioside crude product 3.165g through reclaiming ethanol and concentrating after the vacuum-drying.Prepared rhodioside crude product after polyamide column is further purified, with embodiment 1 described high performance liquid chromatography detect in the rhodioside crude product content of rhodioside be 6.67%.
Embodiment 9: after the 1kg Glossy Privet Fruit is pulverized, adds 5kg60% ethanol, stirs and thorough mixing, soaked 48 hours, reclaim filtrate, extract three times, and merging filtrate, reduced-pressure backflow reclaims ethanol and gets the rhodioside extracting solution; With extracting solution through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, with purified rinse water to the Molish reaction negative, ethanol with 2 times of amounts 25% carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, to the Molish reaction negative, carry out wash-out with the ethanol of 2 times of amounts 25% with purified rinse water, elutriant gets rhodioside crude product 3.206g through reclaiming ethanol and concentrating after the vacuum-drying.Prepared rhodioside crude product after polyamide column is further purified, with embodiment 1 described high performance liquid chromatography detect in the rhodioside crude product content of rhodioside be 7.05%.
Embodiment 10: after the 1kg Glossy Privet Fruit is pulverized, adds 5kg60% ethanol, stirs and thorough mixing, soaked 24 hours, reclaim filtrate, extract three times, and merging filtrate, reduced-pressure backflow reclaims ethanol and gets the rhodioside extracting solution; With extracting solution through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, with purified rinse water to the Molish reaction negative, ethanol with 2 times of amounts 30% carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, to the Molish reaction negative, carry out wash-out with the ethanol of 2 times of amounts 30% with purified rinse water, elutriant gets rhodioside crude product 3.059g through reclaiming ethanol and concentrating after the vacuum-drying.Prepared rhodioside crude product after polyamide column is further purified, with embodiment 1 described high performance liquid chromatography detect in the rhodioside crude product content of rhodioside be 6.82%.
Embodiment 11: after the 1kg Glossy Privet Fruit is pulverized, adds 5kg70% ethanol, stirs and thorough mixing, soaked 48 hours, reclaim filtrate, extract three times, and merging filtrate, reduced-pressure backflow reclaims ethanol and gets the rhodioside extracting solution; With extracting solution through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, with purified rinse water to the Molish reaction negative, ethanol with 2 times of amounts 35% carries out wash-out, elutriant is through reclaiming ethanol and concentrating, again through low-pole AB-8 type absorption with macroporous adsorbent resin 30min, to the Molish reaction negative, carry out wash-out with the ethanol of 2 times of amounts 35% with purified rinse water, elutriant gets rhodioside crude product 2.964g through reclaiming ethanol and concentrating after the vacuum-drying.Prepared rhodioside crude product after polyamide column is further purified, with embodiment 1 described high performance liquid chromatography detect in the rhodioside crude product content of rhodioside be 7.11%.
Claims (4)
1. method for preparing rhodioside, step is as follows:
(1) medicinal material is prepared the rhodioside extracting solution with alcohol solution dipping;
(2) rhodioside extracting solution purifying is prepared the rhodioside crude product;
It is characterized in that said medicinal material is the Chinese medicine Glossy Privet Fruit, adopt macroporous adsorbent resin to carry out purifying.
2. rhodioside preparation method according to claim 1, it is characterized in that: said preparation rhodioside extracting solution is to use the 60-80% alcohol immersion more than 24 hours routinely after Glossy Privet Fruit is pulverized, reclaim filtrate, extract 2-3 time, merging filtrate gets the rhodioside extracting solution behind the recovery ethanol; Said with the purification with macroreticular resin extracting solution be with the rhodioside extracting solution through absorption with macroporous adsorbent resin, purified rinse water to the Molish reaction negative, the 25%-35% ethanol with 2 times of amounts of resin bed volume carries out wash-out again, elutriant is through reclaiming ethanol and concentrating, again by the same method through absorption with macroporous adsorbent resin, purified rinse water to Molish reaction negative, 2 times of amount 25%-35% ethanol elutions, elutriant is through reclaiming ethanol and concentrating, promptly get the rhodioside crude product after the drying, macroporous adsorbent resin is selected from low-pole macroporous adsorbent resin, nonpolar macroporous adsorption resin.
3. rhodioside preparation method according to claim 2, it is characterized in that: the used soak solution of preparation rhodioside extracting solution is 70% ethanol, soak 48h, extract 3 times, used macroporous adsorbent resin is low-pole AB-8 type macroporous resin or nonpolar 1300 type macroporous adsorbent resins during purifying, and elutriant is 30% ethanol.
4. rhodioside preparation method according to claim 3 is characterized in that: used macroporous adsorbent resin is a low-pole AB-8 type macroporous resin during purifying.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392011B (en) * | 2008-11-05 | 2011-05-11 | 江南大学 | Isolation and purification method of natural salidroside |
| CN102492003A (en) * | 2011-11-30 | 2012-06-13 | 四川浩源生物科技有限公司 | Technique for extracting and separating salidroside from glossy privet fruit |
| CN102875614A (en) * | 2012-10-05 | 2013-01-16 | 南通四海植物精华有限公司 | Method for preparing salidroside from rose roots |
| CN103351415A (en) * | 2013-08-02 | 2013-10-16 | 石任兵 | Method for preparing salidrosides with a series of purities from glossy privet fruit |
| CN104542036A (en) * | 2015-01-06 | 2015-04-29 | 湖南中医药大学 | Cultivation method of vegetable containing salidroside and application |
| CN105294789A (en) * | 2015-12-08 | 2016-02-03 | 四川艾丽碧丝制药有限公司 | Preparation method of high-purity salidroside |
| CN106983765A (en) * | 2017-05-15 | 2017-07-28 | 江苏省农业科学院 | A kind of traditional Chinese medicine ingredients prescription for preventing and treating Porcine circovirus desease and its preparation method and application |
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| CN1255121C (en) * | 2003-08-25 | 2006-05-10 | 江苏康缘药业股份有限公司 | Gadol pharmaceutical preparation, method for making same and uses |
| CN1597690A (en) * | 2004-07-21 | 2005-03-23 | 叶利明 | Enrichment method of rhodiola root glycoside compound |
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- 2005-12-22 CN CNB2005101118590A patent/CN100355767C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392011B (en) * | 2008-11-05 | 2011-05-11 | 江南大学 | Isolation and purification method of natural salidroside |
| CN102492003A (en) * | 2011-11-30 | 2012-06-13 | 四川浩源生物科技有限公司 | Technique for extracting and separating salidroside from glossy privet fruit |
| CN102492003B (en) * | 2011-11-30 | 2014-05-07 | 四川浩源生物科技有限公司 | Technique for extracting and separating salidroside from glossy privet fruit |
| CN102875614A (en) * | 2012-10-05 | 2013-01-16 | 南通四海植物精华有限公司 | Method for preparing salidroside from rose roots |
| CN103351415A (en) * | 2013-08-02 | 2013-10-16 | 石任兵 | Method for preparing salidrosides with a series of purities from glossy privet fruit |
| CN104542036A (en) * | 2015-01-06 | 2015-04-29 | 湖南中医药大学 | Cultivation method of vegetable containing salidroside and application |
| CN105294789A (en) * | 2015-12-08 | 2016-02-03 | 四川艾丽碧丝制药有限公司 | Preparation method of high-purity salidroside |
| CN105294789B (en) * | 2015-12-08 | 2018-05-25 | 四川艾丽碧丝制药有限公司 | A kind of preparation method of high-purity salidroside |
| CN106983765A (en) * | 2017-05-15 | 2017-07-28 | 江苏省农业科学院 | A kind of traditional Chinese medicine ingredients prescription for preventing and treating Porcine circovirus desease and its preparation method and application |
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