CN101130561A - Method for producing salidroside and injection containing the same - Google Patents

Method for producing salidroside and injection containing the same Download PDF

Info

Publication number
CN101130561A
CN101130561A CNA2007100755730A CN200710075573A CN101130561A CN 101130561 A CN101130561 A CN 101130561A CN A2007100755730 A CNA2007100755730 A CN A2007100755730A CN 200710075573 A CN200710075573 A CN 200710075573A CN 101130561 A CN101130561 A CN 101130561A
Authority
CN
China
Prior art keywords
rhodioside
filtrate
preparation
alcohol precipitation
value
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.)
Granted
Application number
CNA2007100755730A
Other languages
Chinese (zh)
Other versions
CN101130561B (en
Inventor
张春容
董兆勇
彭红卫
杨伟
赵斌
曾裕建
张宝华
康海歧
李好雨
陈春会
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CHENGDU NUODIKANG BIOLOGICAL PHARMACEUTICAL Co Ltd
Original Assignee
CHENGDU NUODIKANG BIOLOGICAL PHARMACEUTICAL Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by CHENGDU NUODIKANG BIOLOGICAL PHARMACEUTICAL Co Ltd filed Critical CHENGDU NUODIKANG BIOLOGICAL PHARMACEUTICAL Co Ltd
Priority to CN2007100755730A priority Critical patent/CN101130561B/en
Publication of CN101130561A publication Critical patent/CN101130561A/en
Application granted granted Critical
Publication of CN101130561B publication Critical patent/CN101130561B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a making method of rhodiola root glycoside,which comprises the following steps: a. adding water to dissolve crude extract of rhodiola root; adjusting pH value as alkaline; filtering to obtain the filtrate; b. adjusting the filtrate to acid; adsorbing through adsorbing resin; eluting; condensing the eluent; sedimenting the eluent in the alcohol; filtering to obtain the filtrate; c. drying the filtrate through adsorbing resin; adding the dried material into column chromatograph; collecting the chromatographic liquor; d. condensing the chromatographic liquor; doing alcohol sediment; crystallizing. The invention also provides freeze dried and injection of the rhodiola root glycoside with simply and controllably operating condition and high safety, which is easy to accomplish for large scale of industrial manufacturing.

Description

A kind of preparation method of rhodioside, contain the injection of rhodioside
Technical field
The invention provides a kind of preparation method of rhodioside, belong to pharmaceutical field.
Background technology
Root of Kirilow Rhodiola is the root and rhizome of Crassulaceae rhodiola (Rhodiola L.) plant, Rhodida plant has 100 kinds approximately in the whole world, can and abominable and changeable physical environment in grow, for a kind of adaptation former state plant, mainly be distributed in Himalaya mountain area, the northwestward, Asia and North America.China has 80 kinds approximately, is distributed in southwest, northwest, North, Northeast China area more.Discover at present and contain numerous effective constituent such as glycoside in the Root of Kirilow Rhodiola, polyose, organic acid, the matter of mixing, flavonoid, volatile oil, protein, trace element etc., rhodioside is one of its important activeconstituents, has anti-hypoxia, antifatigue, anti-ageing, radioprotective, antitumor, reducing blood-fat and prevents and treats biological actions such as cardiovascular disorder.In view of Root of Kirilow Rhodiola in that so many function and significant curative effect are arranged aspect preventing and curing diseases, make domestic and international many scholars carry out extensive and deep research at the structure and the drug effect of Root of Kirilow Rhodiola single-activity composition one after another.Rhodioside (Salidroside) is the maximum effective constituent of research in the Root of Kirilow Rhodiola, be one of main component of treatment cardiovascular and cerebrovascular diseases, capable of inhibiting cell in calcium ion concn raise, intervene nerve cell apoptosis, neuroprotective cell and treat ischemic brain injury; Radical damage to the rat layer neurocyte has provide protection, can be used for ischemic cerebrovascular; Can obviously increase ischemic animal cardiac muscle content of glycogen, reduce the load effect of heart front and back, help improving and recovering heart function; It is stressed to improve myocardial ischemia oxygen, and myocardial cell injury is had provide protection etc.And toxicological experiment shows, rhodioside toxicity is very little: the mouse subcutaneous injection Root of Kirilow Rhodiola is not caused toxic reaction with 1g/kg; Mouse mainline rhodioside 3g/kg did not see any toxic reaction in continuous five days.
Cardiovascular and cerebrovascular diseases is common disease, frequently-occurring disease clinically.In recent years, raising along with people's living standard, add the aging of demographic structure, its sickness rate is the trend that rises year by year, the exploitation result of treatment medicine of cardiovascular and cerebrovascular diseases has preferably become the focus of current drug research, and increasing clinical study report shows: high purity single component rhodioside has a good application prospect at the treatment treating cardiac and cerebral vascular diseases.
The preparation method of rhodioside is more at present, as: separate in conjunction with macroporous adsorbent resin with solvent extraction, (modern Chinese herbal medicine is studied and is put into practice 2004 the 18th 4 phases of volume for the tough brightness of Tai, the Study on Preparation of highly purified rhodioside with the refining extraction of silicagel column then.)。The rhodioside content that adopts this method to make is low, and can't recycle with silica gel, and the cost height is not suitable for industrialized production.Separate preparation (Ding Chaowu, rhodioside and Root of Kirilow Rhodiola aglycon standard substance preparation method research, analytical test journal, the 16th the 1st phase of volume, 1997.1.25 with the high performance liquid preparative chromatography method with chemistry; ): the product purity height of gained, but the high efficiency chromatography preparation amount is very little, and can't scale operation.In addition polymeric amide, anti-phase macroporous resin, silica gel and four kinds of column chromatographies of dextrane gel are used in combination (Ge Yongchao, Ma Chengyu, Peng Junpeng, the preparation technology of rhodioloside improves, Chinese pharmaceutical chemistry magazine, the 4th 3 phases of volume of September in 1994; ) the preparation rhodioloside, this method separating medium is wide in variety, and the dextrane gel of employing costs an arm and a leg, and silica gel can't recycle, and the whole sepn process time is long, and the cost height is not suitable for industrialized production.Number of patent application: 02100489.7, high-speed countercurrent chromatography prepares rhodioloside, and it is to adopt high-speed countercurrent chromatography to obtain the rhodioloside of 98% purity through twice purifying from the rhodiola root of natural plant vat liquor.But preparation amount is few, and the high speed adverse current chromatogram apparatus expensive can't scale operation.
In order to improve the source of rhodioside, report is arranged, and (wangdan, from the technical study Chinese patent medicine of Glossy Privet Fruit extraction rhodioside, in May, 2006,28 roll up (5) phases etc.) adopt the macroporous resin partition method from Glossy Privet Fruit, to extract rhodioside, as: extract rhodioside in the Glossy Privet Fruit, number of patent application: 200510111859.0, denomination of invention: a kind of method for preparing rhodioside is to adopt macroporous resin purification technology partition method to extract the method for rhodioside crude product in the Glossy Privet Fruit.This method is Glossy Privet Fruit to be pulverized in the lixiviate of 60-80% ethanol get the rhodioside extracting solution, with it through low-pole AB-8 type macroporous resin adsorption, earlier with purified rinse water, again through the 25-35% ethanol elution, collect elutriant reclaim ethanol and concentrate after again through low-pole AB-8 type macroporous resin adsorption, through purified rinse water, the 25-35% ethanol elution reclaims ethanol and concentrates promptly.This method adopts ethanol for extracting solvent, preparation be the rhodioside crude product.Though the Glossy Privet Fruit wide material sources, cost of material is cheap, and the content of the rhodioside that is obtained and purity are all very low, and the content of rhodioside is not higher than 10%.
Application number: 200510026830.2, denomination of invention: " two-step resin method for preparing salidrose ", disclose and from neutral red red-spotted stonecrop crude extract, separated the preparation high-purity salidroside, it with Root of Kirilow Rhodiola crude extract temperature 20~90 ℃ water stirring and dissolving, filter, it is 1~5 that filtrate is regulated pH, flow through adsorption resin column under the normal temperature, use acetone, low-carbon alcohol or acetate esters organic solvent wash-out, concentrate eluant adds in the chromatography column and carries out chromatography under the normal temperature, chromatographic solution concentrates evaporate to dryness, add low-carbon alcohol or acetate esters organic solvent heating for dissolving, filter concentrated filtrate, separate out crystallization, filter high-purity salidroside.In the preparation method, it is 1~5 that the rhodioside essence extract is regulated pH, flows through adsorption resin column under the normal temperature, cross the rate difficulty, adsorption rate is low, and the rhodioside yield for preparing is low, exploitativeness is poor, is difficult to obtain highly purified rhodioside, is unfavorable for the requirement of industrialized production.
Summary of the invention
The invention provides a kind of new preparation method of rhodioside.The present invention also provides the injection that contains rhodioside.
The invention provides a kind of preparation method of rhodioside, it comprises the steps:
A, with the Root of Kirilow Rhodiola crude extract, pH value is regulated for alkaline in the back that is dissolved in water, and filters to get filtrate;
B, adjusting filtrate are to acid, and polymeric adsorbent adsorbs, wash-out, and elutriant concentrates, alcohol precipitation, filters to get filtrate;
C, with b step filtrate by polymeric adsorbent absorption oven dry, the oven dry back adds column chromatography, collects chromatographic solution;
D, chromatographic solution concentrate, alcohol precipitation, crystallization.
Wherein, b, the described resin of c step are non-polar resin, as, XAD series macroporous adsorbent resin: XAD-4, XAD-16, XAD-1600; HZ macroporous adsorbent resin HZ-816; H-20, CG161 etc., the resin that b, c step are used can be identical, also can be inequality.B, c step preferred resin are macroporous adsorbent resin HZ-816.
Wherein, it is 50~60 ℃ that described a step adds water temp, transfers alkali pH value 8~12.
Described b step transfers acid ph value to be: 1~3; Elutriant is: 10~50% ethanol elution; Described alcohol precipitation is the dehydrated alcohol precipitation.
The described column chromatography of step c is 5%~35% ethanol elution.
The described alcohol precipitation of steps d is the dehydrated alcohol precipitation.
B, the more same kind solvent of the described dehydrated alcohol of d step, safer, because acetate esters is flammable, its steam and air form explosive mixture; In addition, adopt anhydrous second to filter and obtain clear filtrate, filtrate adds resin absorption back oven dry fully, because boiling point is low, volatilization is fast, has eliminated organic residual quantity, has guaranteed the quality of product to greatest extent.
The present invention also provides the rhodioside of above-mentioned preparation method's preparation.
The rhodioside of the present invention's preparation calculates with the rhodioside dry product, and its content is 90%~99%.
Figure A20071007557300061
Rhodioside molecular formula: C 14H 20O 7, molecular weight: 300.31.
The invention provides a kind of Hongjingtian glycoside freeze dried powder injection agent, it is that the rhodioside that is prepared by described method is that activeconstituents is prepared from.
Hongjingtian glycoside freeze dried powder injection agent of the present invention, it is by following weight:
2~200 parts of rhodiosides, 0~80 part in N.F,USP MANNITOL.
The invention provides a kind of rhodiola root glycosides injection, it is to be that activeconstituents is prepared from by rhodioside.
It is to be prepared from by following weight percentages: 2~200 parts of rhodiosides, oxidation inhibitor: sodium bisulfite, 0.5~2 part of consumption; Or Sodium Pyrosulfite, 0.5~5 part of consumption; The pH regulator agent: sodium hydroxide, regulate pH value 4.5~6.5.
Structure according to rhodioside contains phenolic hydroxyl group, and is oxidized easily, in order to guarantee its stability, adds oxygenant and is used as being used for intravenous hydro-acupuncture preparation.
Preparation method of the present invention at first transfers alkali, can remove in the Root of Kirilow Rhodiola crude product most of impurity as flavonoid, the impurity such as matter, protein, polyose of mixing.After adopting resin absorption and chromatography, the yield of rhodioside improves several times, and more efficiently minimizing more helps the recycling of resin to the infringement of resin; Also reduce simultaneously the consumption of elutriant greatly, reduced cost; The rhodioside purity and the content of preparation all can reach 90%~99%, operational condition simple controllable of the present invention, and working method is easy to implement, and preparation amount is big, helps industrialized production more.
Embodiment
The preparation method of embodiment 1 rhodioside of the present invention
The Root of Kirilow Rhodiola crude extract is added in 50 ℃ of water, and stirring and dissolving is regulated pH value=11, filtration obtains clear filtrate, filtrate is regulated filtrate pH value=2, adsorbs with the HZ-816 polymeric adsorbent, uses 10% ethanol elution then, concentrate eluant is fully to doing, add the dehydrated alcohol precipitation, filter and obtain clear filtrate, filtrate adds the back oven dry fully of HZ-816 resin absorption, HZ-816 polymeric adsorbent after the oven dry is joined in the chromatography column and (is called sample column), get elutriant with 5% ethanol elution.Elutriant is directly gone up on another root chromatography column (being called chromatography column) carry out chromatography, chromatographic solution is concentrated into dried, add anhydrous alcohol solution, filter, concentrated filtrate is placed to separating out crystallization, crystallization, drying obtains highly purified rhodioside goods, and the content of these rhodioside goods reaches 98%.
The preparation method of embodiment 2 rhodiosides of the present invention
The Root of Kirilow Rhodiola crude extract is added in 60 ℃ of water, and stirring and dissolving is regulated pH value=12, filtration obtains clear filtrate, filtrate is regulated filtrate pH value=3, adsorbs with the HZ-816 polymeric adsorbent, uses 50% ethanol elution then, concentrate eluant is fully to doing, add the dehydrated alcohol precipitation, filter and obtain clear filtrate, filtrate adds the back oven dry fully of HZ-816 resin absorption, HZ-816 polymeric adsorbent after the oven dry is joined in the chromatography column and (is called sample column), get elutriant with 35% ethanol elution.Elutriant is directly gone up on another root chromatography column (being called chromatography column) carry out chromatography, chromatographic solution is concentrated into dried, add anhydrous alcohol solution, filter, concentrated filtrate is placed to separating out crystallization, crystallization, drying obtains highly purified rhodioside goods, and the content of these rhodioside goods reaches 92%.
The preparation method of embodiment 3 rhodiosides of the present invention
The Root of Kirilow Rhodiola crude extract is added in 55 ℃ of water, and stirring and dissolving is regulated pH value=8, filtration obtains clear filtrate, filtrate is regulated filtrate pH value=1, adsorbs with the HZ-816 polymeric adsorbent, uses 20% ethanol elution then, concentrate eluant is fully to doing, add the dehydrated alcohol precipitation, filter and obtain clear filtrate, filtrate adds the back oven dry fully of HZ-816 resin absorption, HZ-816 polymeric adsorbent after the oven dry is joined in the chromatography column and (is called sample column), get elutriant with 5% ethanol elution.Elutriant is directly gone up on another root chromatography column (being called chromatography column) carry out chromatography, chromatographic solution is concentrated into dried, add anhydrous alcohol solution, filter, concentrated filtrate is placed to separating out crystallization, crystallization, drying obtains highly purified rhodioside goods, and the content of these rhodioside goods reaches 94%.
The foundation that the pH value is selected in embodiment 4 extraction steps of the present invention
1, a step accent alkali pH is 8,9,10,11,12, selects between 10~12.Concrete correlation data is as follows:
Different pH values are to the influence of rhodioside yield
pH 8 9 10 11 12
The rhodioside yield 80% 85% 90.5% 92% 92%
When pH less than 7 the time, filtration difficulty, yield are extremely low.
Interpretation of result: selecting pH value be between the 8-9 time, the filtered liquid muddiness, and be easy to obstruction during filtration, filtration time is long, but yield can reach 80%; The pH value is between the 10-12, and yield can reach more than 90%, and the pH value is that 11 o'clock filtration velocity increase to maximum, and filtration velocity changes not obvious when pH increases to 12.So select the pH value between 10-12, preferred 11.
2, b step acid adjustment parameter is selected:
Different pH values are to the influence of rhodioside polymeric adsorbent situation
pH 1 2 3 4 5 6
Adsorptive capacity (mg) adsorption rate (%) 53.5 35.7 72.8 48.5 34.8 23.2 33.2 22.1 37.7 25.1 27.6 18.4
Q=(Co-Cr)×V/W
In the formula: Q is adsorptive capacity (mg/g); Co is original liquid concentration (mg/ml); Cr is absorption residual concentration (mg/ml); V is adsorption liquid volume (ml); W is weight resin (g).
The rhodioside dissociation degree is reduced, and the ratio that the big glycosides of red scape is molecular state increases, and helps by resin adsorbed.PH is the adsorptive capacity maximum of 2 o'clock rhodiosides.The purpose of b step acid adjustment is: the rhodioside dissociation degree is reduced, and the ratio that rhodioside is molecular state increases, and helps by resin adsorbed.PH is the adsorptive capacity maximum of 2 o'clock rhodiosides.
The acid adjustment of above-mentioned accent alkali must be carried out in order, because rhodioside solution itself is acid, transferring alkali is for removal of impurities, and acid adjustment is to be convenient to resin absorption in order to make rhodioside be the free state again.
Embodiment 5 salidroside injection agent Study on Forming
One, the screening of supplementary product kind:
Auxiliary material:, the auxiliary material of preparation is selected according to the structural formula of rhodioside itself:
The selection of antioxidant is investigated index: the content of rhodioside, solution colour.
Investigation method: by prescription proportional arrangement injection liquid, regulate pH to 4.5~6.5, according to the form below adds 0.05% dissimilar antioxidant, packing, gland, place hot water to boil 10 hours, the observation solution colour (" an appendix XI of Chinese pharmacopoeia version in 2005 A), the photograph high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 D).Measure the content of rhodioside.(when initial experiment, the content of rhodioside is 50mg/ml) sodium bisulfite, consumption 0.05~0.2%; Sodium Pyrosulfite, consumption 0.05~0.5%;
Disodium ethylene diamine tetraacetate: 0.03~0.05%; Thiocarbamide 0.05~0.1%.
The screening table of supplementary product kind
The selection of antioxidant Kind Solution colour Rhodioside content (mg/ml)
Do not add antioxidant Near Y-2 45
Sodium bisulfite Be shallower than Y-1 50
Sodium Pyrosulfite Be shallower than Y-1 49
Thiocarbamide Be shallower than Y-1 45
Disodium ethylene diamine tetraacetate Be shallower than Y-1 47
When not adding antioxidant, the content of rhodioside changes, and color is yellow partially, illustrates itself may part oxidized.Table has been selected auxiliary material industry sodium pyrosulfate, Sodium Pyrosulfite, preferred sodium bisulfite thus.
The selection experimental program of supplementary product consumption
The name of an article Consumption (%)
Sodium bisulfite 0.05 0.1 0.15 0.2
Color Be shallower than Y-1 Be shallower than Y-1 Be shallower than Y-1 Be shallower than Y-1
Rhodioside content (mg/ml) 50 50 50 50
Y-1, Y-2 refer to the depth of yellow color.Regulation according to national contrasting colour: yellow is divided into 7 kinds of gradients, is 1,2,3,4,5,6,7 from shallow to deep, stipulates that the color of rhodiola root glycosides injection of the present invention must be less than Y-3, and is qualified by colorimetry rhodioside of the present invention as can be known, should be Y-1, Y-2.According to injection supplementary product consumption being required is the few more good more principle of auxiliary material, in conjunction with the content situation of rhodioside behind the adding antioxidant, preferred sodium bisulfite.
The preparation technology of embodiment 6 rhodioside powder injection:
1) gets rhodioside 54.23g (content 92.2%), add 800ml water for injection, be stirred to dissolving fully;
2) with sodium hydroxide adjust pH 4.5;
3) add N.F,USP MANNITOL 40g again, stir and make dissolving, add the injection water to 1000mL;
4) soup adds the 0.25g gac, and little insulation 10 minutes of boiling is put cold;
5) millipore filtration with 0.45 μ m, 0.22 μ m filters, and filtrate filtrate is filled to 5ml control antibiotic glass bottle, and every bottle of 1ml adds a cover treated butyl rubber plug;
6) lyophilize promptly, specification is the 50mg/ bottle.
The preparation technology of embodiment 7 rhodioside powder injection:
1) gets rhodioside 209.42g (content is 95.5%), add 800ml water for injection, be stirred to dissolving fully;
2) with sodium hydroxide adjust pH 5.8;
3) soup adds the 1g gac, and little insulation 10 minutes of boiling is put cold;
4) millipore filtration with 0.45 μ m, 0.22 μ m filters, and filtrate filtrate is filled to 5ml control antibiotic glass bottle, and every bottle of 1ml adds a cover treated butyl rubber plug;
5) lyophilize promptly, specification is the 200mg/ bottle.
The preparation technology of embodiment 8 rhodioside powder injection:
1) gets rhodioside 2.14g (content is 93.5%), add 800ml water for injection, be stirred to dissolving fully;
2) with sodium hydroxide adjust pH 6.5;
3) add the N.F,USP MANNITOL 80g of recipe quantity again, stir and make dissolving, add the injection water to 1000mL;
4) soup adds the 0.5g amount and adds gac, and little insulation 10 minutes of boiling is put cold;
5) millipore filtration with 0.45 μ m, 0.22 μ m filters, and filtrate filtrate is filled to 5ml control antibiotic glass bottle, and every bottle of 1ml adds a cover treated butyl rubber plug;
6) lyophilize promptly, specification is the 2mg/ bottle.
The preparation technology of embodiment 9 rhodioside powder injection
Get rhodioside 218.58g (content is 91.5%), N.F,USP MANNITOL 80g, the method preparation of pressing embodiment 8;
Embodiment 10 salidroside injection agent
1) gets rhodioside 215.98g (content is 92.6%), add 800ml water for injection, be stirred to dissolving fully;
2) with sodium hydroxide adjust pH 5.0;
3) the sodium bisulfite 0.6g that adds again stirs and makes dissolving, adds the injection water to 1000mL;
4) soup adds the 1g gac, and little insulation 10 minutes of boiling is put cold;
5) millipore filtration with 0.45 μ m, 0.22 μ m filters, and filtrate filtrate is filled to 5ml control antibiotic glass bottle, every bottle of 1ml, and 100 ℃ of sterilization 30min, promptly.
The preparation technology of embodiment 11 rhodiola root glycosides injections:
1) gets rhodioside 20.2g (content is 99%), add 800ml water for injection, be stirred to dissolving fully;
2) with sodium hydroxide adjust pH 5.6;
3) the sodium bisulfite 0.5g that adds again stirs and makes dissolving, adds the injection water to 1000mL;
4) soup adds the 0.5g gac, and little insulation 10 minutes of boiling is put cold;
5) millipore filtration with 0.45 μ m, 0.22 μ m filters, and filtrate filtrate is filled to 5ml control antibiotic glass bottle, every bottle of 1ml, and 100 ℃ of sterilization 30min, promptly.
The preparation technology of embodiment 12 rhodiola root glycosides injections:
1) gets rhodioside 2.08g (content is 96.1%), add 800ml water for injection, be stirred to dissolving fully;
2) with sodium hydroxide adjust pH 4.9;
3) the Sodium Pyrosulfite 0.5g that adds again stirs and makes dissolving, adds the injection water to 1000mL;
4) soup adds the 0.5g gac, and little insulation 10 minutes of boiling is put cold;
5) millipore filtration with 0.45 μ m, 0.22 μ m filters, and filtrate filtrate is filled to 5ml control antibiotic glass bottle, every bottle of 1ml, and 100 ℃ of sterilization 30min, promptly.
The preparation technology of embodiment 13 rhodiola root glycosides injections:
1) gets rhodioside 10.30g (content is 97.1%), add 800ml water for injection, be stirred to dissolving fully;
2) with sodium hydroxide adjust pH 5.2;
3) the sodium bisulfite 2g that adds again stirs and makes dissolving, adds the injection water to 1000mL;
4) soup adds the 0.25g gac, and little insulation 10 minutes of boiling is put cold;
5) millipore filtration with 0.45 μ m, 0.22 μ m filters, and filtrate filtrate is filled to 5ml control antibiotic glass bottle, every bottle of 1ml, and 100 ℃ of sterilization 30min, promptly.

Claims (10)

1. the preparation method of a rhodioside, it comprises the steps:
A, with the Root of Kirilow Rhodiola crude extract, pH value is regulated for alkaline in the back that is dissolved in water, and filters to get filtrate;
B, adjusting filtrate pH are to acid, and polymeric adsorbent adsorbs, wash-out, and elutriant concentrates, alcohol precipitation, filters to get filtrate;
C, with b step filtrate by polymeric adsorbent absorption oven dry, the oven dry back adds column chromatography, collects chromatographic solution;
D, chromatographic solution concentrate, alcohol precipitation, crystallization.
2. the preparation method of rhodioside according to claim 1, it is characterized in that: it is 50~60 ℃ that described a step adds water temp, transfers alkali pH value 8~12.
3. the preparation method of rhodioside according to claim 1 is characterized in that: described b step transfers acid ph value to be: 1~3; Elutriant is: 10~50% ethanol elutions; Described alcohol precipitation is the dehydrated alcohol precipitation.
4. the preparation method of rhodioside according to claim 1, it is characterized in that: the described column chromatography of step c is 5%~35% ethanol elution.
5. the preparation method of rhodioside according to claim 1 is characterized in that: the described alcohol precipitation of steps d is the dehydrated alcohol precipitation.
6. the rhodioside of each described preparation method preparation of claim 1-5.
7. Hongjingtian glycoside freeze dried powder injection agent, it is to be that activeconstituents is prepared from by the described rhodioside of claim 6.
8. Hongjingtian glycoside freeze dried powder injection agent according to claim 7 is characterized in that: it is to be prepared from by the following weight proportion raw material:
2~200 parts of rhodiosides, 0~80 part in N.F,USP MANNITOL.
9. rhodiola root glycosides injection, it is to be that activeconstituents is prepared from by the described rhodioside of claim 6.
10. rhodiola root glycosides injection according to claim 1 is characterized in that: it is to be prepared from by the following weight proportion raw material: 2~200 parts of rhodiosides, oxidation inhibitor: sodium bisulfite, 0.5~2 part of consumption; Or Sodium Pyrosulfite, 0.5~5 part of consumption; The pH regulator agent: sodium hydroxide, regulate pH value 4.5~6.5.
CN2007100755730A 2007-08-10 2007-08-10 Method for producing salidroside and injection containing the same Active CN101130561B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2007100755730A CN101130561B (en) 2007-08-10 2007-08-10 Method for producing salidroside and injection containing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2007100755730A CN101130561B (en) 2007-08-10 2007-08-10 Method for producing salidroside and injection containing the same

Publications (2)

Publication Number Publication Date
CN101130561A true CN101130561A (en) 2008-02-27
CN101130561B CN101130561B (en) 2010-10-06

Family

ID=39127982

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2007100755730A Active CN101130561B (en) 2007-08-10 2007-08-10 Method for producing salidroside and injection containing the same

Country Status (1)

Country Link
CN (1) CN101130561B (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101974045A (en) * 2010-10-19 2011-02-16 康美药业股份有限公司 Method for preparing salidroside
CN102382152A (en) * 2011-10-11 2012-03-21 康美药业股份有限公司 Method for preparing salidroside
CN103351416A (en) * 2013-08-02 2013-10-16 福建中医药大学 New crystal form A of salidroside and preparation method thereof
CN104017036A (en) * 2014-06-11 2014-09-03 福建中医药大学 Novel crystal form of rhodioloside and preparation method of novel crystal form
CN104523810A (en) * 2014-12-17 2015-04-22 通化玉圣药业有限公司 Hyperthermic devitalization extraction method of rhodiola rosea injection
CN108329363A (en) * 2018-01-30 2018-07-27 合肥华恒生物工程有限公司 The minimizing technology of quinhydrones in alpha-arbutin conversion fluid
CN108434192A (en) * 2018-05-15 2018-08-24 安徽益草堂中药饮片有限公司 A kind of preparation method of the rhodiola root prepared slices of Chinese crude drugs
CN110420222A (en) * 2019-07-31 2019-11-08 杭州荣泽生物科技有限公司 A kind of rhodioside joint mesenchymal stem cell injection and preparation method thereof for cardiomyopathy
CN112194689A (en) * 2020-09-27 2021-01-08 湖南朗林生物资源股份有限公司 Method for extracting effective active ingredients of rhodiola rosea

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1880326B (en) * 2005-06-16 2010-11-03 周晓明 Two-step resin method for preparing salidrose

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101974045A (en) * 2010-10-19 2011-02-16 康美药业股份有限公司 Method for preparing salidroside
CN101974045B (en) * 2010-10-19 2013-11-20 康美药业股份有限公司 Method for preparing salidroside
CN102382152A (en) * 2011-10-11 2012-03-21 康美药业股份有限公司 Method for preparing salidroside
CN103351416A (en) * 2013-08-02 2013-10-16 福建中医药大学 New crystal form A of salidroside and preparation method thereof
CN104017036A (en) * 2014-06-11 2014-09-03 福建中医药大学 Novel crystal form of rhodioloside and preparation method of novel crystal form
CN104523810A (en) * 2014-12-17 2015-04-22 通化玉圣药业有限公司 Hyperthermic devitalization extraction method of rhodiola rosea injection
CN104523810B (en) * 2014-12-17 2018-01-23 通化玉圣药业有限公司 Gadol injection high-temperature inactivation extracting method
CN108329363A (en) * 2018-01-30 2018-07-27 合肥华恒生物工程有限公司 The minimizing technology of quinhydrones in alpha-arbutin conversion fluid
CN108434192A (en) * 2018-05-15 2018-08-24 安徽益草堂中药饮片有限公司 A kind of preparation method of the rhodiola root prepared slices of Chinese crude drugs
CN110420222A (en) * 2019-07-31 2019-11-08 杭州荣泽生物科技有限公司 A kind of rhodioside joint mesenchymal stem cell injection and preparation method thereof for cardiomyopathy
CN112194689A (en) * 2020-09-27 2021-01-08 湖南朗林生物资源股份有限公司 Method for extracting effective active ingredients of rhodiola rosea
CN112194689B (en) * 2020-09-27 2022-08-30 湖南朗林生物资源股份有限公司 Method for extracting effective active ingredients of rhodiola rosea

Also Published As

Publication number Publication date
CN101130561B (en) 2010-10-06

Similar Documents

Publication Publication Date Title
CN101130561B (en) Method for producing salidroside and injection containing the same
CN110845328B (en) Method for preparing high-purity carnosic acid from rosemary ointment byproducts
US6267995B1 (en) Extract of Lepidium meyenii roots for pharmaceutical applications
CN111039761B (en) Method for purifying cannabidiol
CN1847237A (en) Ginkgo leaf extract and production process of separating high purity effective component of the extract
CN101862385B (en) Sanguisorba saponins and preparation method of sanguisorbin I
CN102875562A (en) Method for preparing psoralen and isopsoralen or extract containing psoralen and isopsoralen
CN105859803B (en) A kind of preparation method of galloyl glucose
CN105503786A (en) Secolignan compound-nettle secolignan glucoside E and preparation method thereof
CN108409805B (en) Separation and purification method of delphinidin-3-O-galactoside and application thereof
WO2012061984A1 (en) Method for preparing albiflorin and paeoniflorin
CN108409806B (en) Method for separating and preparing petunidin-3-O-glucoside
CN107602642B (en) Method for extracting and purifying trachelospermin from safflower seed
CN108285443B (en) Refining method of silybin
CN109369752B (en) Method for extracting kaempferol galactose type compound from Nanshan tea
CN105330707B (en) It is a kind of while separating the Industrialized processing technique of ponticin and Rhapontin, deoxy-
CN109541063B (en) Method for extracting kaempferol glucoside compounds from Nanshan tea
CN109369750B (en) Method for extracting kaempferol galactoside compounds from Nanshan tea
CN109265493B (en) Kaempferol compound and extraction method thereof
CN114057826B (en) Preparation method of reference substance of toosendanin
CN109490448A (en) A kind of preparation method of digoxin standard substance
CN115466256B (en) Method for extracting, separating and purifying matrine and sophoridine from sophora alopecuroide
JPS6227074B2 (en)
CN106977525B (en) A kind of mibemycin preparation method
CN101475617B (en) Refining method for gardenin for injection

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant