CN101396381B - Valerian extract and preparation method and use thereof - Google Patents
Valerian extract and preparation method and use thereof Download PDFInfo
- Publication number
- CN101396381B CN101396381B CN2007101754415A CN200710175441A CN101396381B CN 101396381 B CN101396381 B CN 101396381B CN 2007101754415 A CN2007101754415 A CN 2007101754415A CN 200710175441 A CN200710175441 A CN 200710175441A CN 101396381 B CN101396381 B CN 101396381B
- Authority
- CN
- China
- Prior art keywords
- extract
- rhizoma
- radix valerianae
- extraction
- valerian
- 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.)
- Expired - Fee Related
Links
Images
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a setwall extract with hypnotic sedative activity and the preparation thereof and also comprises the application of the extract in the pharmacy field. The extract essentially consists of setwall naphtha, valerienic acid, total valepotriate, etc. The pharmacodynamical experiment shows that the setwall extract made by the technology has the marked pharmacological actions of mitigation, hypnosis, anti-depression, spasmolysis, analgesis, the regulation of blood fat, anti-tumor, antibiosis, antivirus and the like and can be developed into medicine or food with health care function.
Description
Technical field
The present invention relates to a kind of plant extract and its production and use, particularly a kind of Rhizoma et radix valerianae extract and its production and use.
Background technology
Rhizoma et radix valerianae is a Valerianaceae valeriana herbaceos perennial, mainly contain compositions such as monoterpenes, sesquiterpenoids, iridoids, alkaloids, flavonoid, lignanoids, have pharmacological actions such as tranquilizing soporific, antidepressant, spasmolysis and analgesia, blood lipid regulation, antitumor, antibiotic, antiviral.It as a kind of calmness of gentleness, calm the nerves, hypnotic, the applicating history of centuries has been arranged in Europe, its medical value comes into one's own in the world.
Because clinical tranquilizing soporific class Western medicine commonly used has in various degree drug dependence and addiction, select the plant amedica treatment to become a kind of trend.Rhizoma et radix valerianae has become one of the highest natural drug of American-European countries's sales volume at present.
The existing patent of method that Rhizoma et radix valerianae is extracted mostly is the method for solvent extraction greatly, the complex process that patent US3869476 (Therapeutically active isovaleric acid esters) preparation general valerianin uses, step is various, time-consuming is long, and use the big organic solvent of a large amount of toxicity such as benzene and acetic acid, health to operator is harmful, big for environment pollution.Patent CN1396166A (denomination of invention is a kind of new method for preparing general valerianin) has introduced and has used the Petroleum ether extraction general valerianin, but has lost the active component valerian naphtha.Patent CN1337255A (denomination of invention is a kind of preparation method of Rhizoma et radix valerianae extract) is the method that adopts ethanol percolate extraction.Patent CN1370586A (denomination of invention is the medical usage of northern Rhizoma et radix valerianae extractive with organic solvent) has introduced methanolic extract and as the purposes of calming soporific class medicine.Patent CN1475490A is that the method that adopts supercritical extraction and organic solvent extraction to combine is extracted valerian naphtha and general valerianin, the method complexity, need with supercritical extraction volatile oil and two leaching process of organic solvent extraction general valerianin, and the method for organic solvent percolation is extracted the general valerianin composition, the percolation liquid measure is big, and decompression and solvent recovery needs the heating process of long period.General valerianin becomes to belong to iridoids, and structural instability, chemical property are extremely active, and the easy recurring structure of long-time heating changes.
Summary of the invention
The object of the invention is to provide a kind of Rhizoma et radix valerianae extract; Another purpose of the present invention is to provide this preparation method of extract; The present invention also aims to provide this extract to have application in the medicine of sedative-hypnotic effect in preparation.
The present invention seeks to be achieved through the following technical solutions.
Rhizoma et radix valerianae extract of the present invention one of can be by the following method be prepared from:
A. the static entrainer method of adding: with any coarse powder that is ground in the valerian, cross 10～20 mesh sieves, place extraction kettle, add entrainer, the mass ratio of medical material and entrainer is 1: 0.5～1.5 (W/W), carry out static extracting 0.5～8 hour with 7.0～45Mpa, 30～80 ℃ of conditions, carry out dynamic extraction 30min～8h again, be dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the entrainer decompression and solvent recovery in the extract.
B. dynamically add the entrainer method: any coarse powder that is ground in the valerian, cross 10～20 mesh sieves, place extraction kettle to extract, extracting pressure is 7.0～45Mpa, 30～80 ℃ of extraction temperature, be 1%～50% of carbon dioxide by mass percentage to the amount that wherein adds entrainer, extract time 30min～8h, be dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the entrainer decompression and solvent recovery in the extract.
C. the static and dynamic entrainer method of adding: with any coarse powder that is ground in the valerian, cross 10～20 mesh sieves, place extraction kettle, add entrainer, the mass ratio of medical material and entrainer is 1: 0.25～1.25 (W/W), earlier carry out static extracting 30min～8h with 7.0～45Mpa, 30～80 ℃, dynamically add entrainer again, this moment, the amount of entrainer was 1%～20% of carbon dioxide by mass percentage, under identical extracting pressure and temperature conditions, extracted 0.5～2 hour, and be dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the entrainer decompression and solvent recovery in the extract.
Rhizoma et radix valerianae extract of the present invention is preferably as follows the preparation of one of method:
A. the static entrainer method of adding: with any coarse powder that is ground in the valerian, cross 10 mesh sieves, place extraction kettle, add entrainer, the mass ratio of medical material and entrainer is 1: 1.25, carries out static extracting 2 hours with 30Mpa, 40 ℃ of conditions; Carry out dynamic extraction 2h again, be dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the entrainer decompression and solvent recovery in the extract.
B. dynamically add the entrainer method: any coarse powder that is ground in the valerian, cross 10 mesh sieves, place extraction kettle to extract, extracting pressure is 25Mpa, 40 ℃ of extraction temperature, be 10% of carbon dioxide by mass percentage to the amount that wherein adds entrainer, extract time 2h, be dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the entrainer decompression and solvent recovery in the extract.
C. static and dynamically add the entrainer method: with any coarse powder that is ground in the valerian, cross 10 mesh sieves, place extraction kettle, add entrainer, the mass ratio of medical material and entrainer is 1: 1.25, and elder generation carried out static extracting 1 hour with 25Mpa, 40 ℃; Dynamically add entrainer again, this moment, the amount of entrainer was 5% of carbon dioxide by mass percentage, extracted 2h under identical extracting pressure and temperature conditions, was dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the entrainer decompression and solvent recovery in the extract.
Described entrainer is solution such as the ethanol, methanol, normal propyl alcohol, isopropyl alcohol, n-butyl alcohol, n-amyl alcohol, isoamyl alcohol, acetone, ethyl acetate, ether, petroleum ether, chloroform of various concentration.
The present invention is used for extracting the valerian of Rhizoma et radix valerianae extract, is meant all plants that contain valerian naphtha and general valerianin.
The unit of described mass ratio is: g/g or w/w.
The unit of described mass percent is w/w% or g/g%, and the amount of entrainer is relative value, depends on the amount of carbon dioxide, and the volume of carbon dioxide can be read from instrument, is converted into weight to be:
In the computing formula: the atmospheric pressure of supposing the same day is an atmospheric pressure: 1.01 * 10
5Pascal
V
(CO2)Expression CO2 volume (cubic meter),
T represent Celsius temperature (℃),
(t+273.15) the expression Celsius temperature is converted into absolute temperature (K).
Rhizoma et radix valerianae extract of the present invention can add conventional adjuvant by practice of pharmacy, is that active component is made single preparations of ephedrine with this extract, or makes the medicine composition that contains the said extracted thing.Dosage form comprises: tablet, soft capsule, oral liquid, drop pill, microcapsule, granule, injection, injectable powder, infusion solution or fat milk injection.Wherein the Rhizoma et radix valerianae extract existence can be solid or liquid, and administering mode can be oral, intramuscular injection or intravenous injection.Its purposes can be that medicine also can be a health food.
The supercritical extraction method that process using of the present invention increases a small amount of entrainer once extracts valerian naphtha and general valerianin, do not need to increase the step of with an organic solvent extracting, and the consumption of entrainer is few, and it is short heat time heating time therefore to reclaim solvent, the active component general valerianin is destroyed few.
Experiment shows that Rhizoma et radix valerianae extract of the present invention has sedation, can be used for being prepared into medicine or health food with sedation.
Following experimental example and embodiment are used to further specify the present invention, but are not limited to constitute the qualification to the claimed scope of the present invention.
The Study on Extraction Method of experimental example 1 valerian naphtha
1, steam distillation: get Rhizoma et radix valerianae coarse powder 200g, put in the volatile oil extractor, add water 1000ml, extracting 12h volatile oil is not continuously increasing, and gets volatile oil 0.50g, calculates oil yield, is about 0.25%.
2, ethanol extraction method: get Rhizoma et radix valerianae coarse powder 200g, with 95% alcohol reflux 3 times, quantity of solvent is respectively 5 times, 4 times, 3 times, and extraction time is respectively 2h, 1h, 1h, merge extractive liquid,, and being evaporated to does not have the alcohol flavor.The weighing extract heavily is 19.34g, and calculating yield is 9.67%.
3, supercritical extraction: get Rhizoma et radix valerianae coarse powder 200g, place extraction kettle to extract, extracting pressure is 30Mpa, and 35 ℃ of extraction temperature extract time 2h, are dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still, resolve pressure 6.0Mpa, 40 ℃ of desorption temperatures are resolved time 30min, get valerian naphtha 4.32g.Calculating oil yield is 2.16%.
Table 1 contrast distinct methods extracts the oil yield and the extract character of valerian naphtha
| Extracting method | Extraction time (h) | Oil yield (%) | Character |
| Steam distillation ethanol extraction supercritical extraction | ?12?4?2 | 0.25％ 9.67％ 2.16％ | Pale yellow oily liquid body sepia extractum yellow oily liquid |
The volatile oil yield of steam distillation extraction is low as seen from the above table; Though ethanol extraction yield height, impurity is too many, and extract is solid, contain in the extract a large amount of in low polar material; And the volatile oil yield height that the method for supercritical extraction is extracted, impurity is few, and extraction time is short, and it is low to extract temperature, can not destroy the thermal sensitivity composition, is particularly suitable for the extraction of volatile oil.
The sedation research of the extracting solution of experimental example 2 Rhizoma et radix valerianae distinct methods preparation
Kunming mouse 18～22g, male and female half and half, random packet, 20 every group.To make the suspension that contains 0.5% tween 80 of variable concentrations by the valerian naphtha extract that embodiment 1 described method makes.And be blank with 0.5% tween 80 solution.Behind drug oral gastric infusion 30min, lumbar injection pentobarbital sodium 50mg/kg, with righting reflex loss to recovery time as the length of one's sleep.
Table 2 Rhizoma et radix valerianae extract is to the pentobarbital sodium influence of the length of one's sleep
| Group | Dosage (gkg -1) | Administering mode | The length of one's sleep (min) | The P value |
| Blank steam distillation ethanol extraction supercritical extraction | ?0.2?0.2?0.2 | ig ig ig ig | 71.5±24.4 95.8±30.6 82.5±25.4 116.3±34.1 | ＜0.05 ＜0.05 ＜0.01 |
From last table as seen, the extractive of volatile oil of the method for supercritical extraction preparation sleep time expand, is the longest; The supercritical extraction group has been compared significant difference with the ethanol extraction group length of one's sleep, and the extract sleep time expand weak point of the method preparation of 95% ethanol extraction may be too high relevant with its impurity content; Extractive of volatile oil sleep time expand of the method for steam distillation preparation, is also longer, but the productive rate of this method volatile oil is too low.
The technical study of test example 3 supercritical fluid extraction valerian naphthas
The 1 static entrainer method of adding:
(1) influence of extracting pressure
Get the Rhizoma et radix valerianae coarse powder (all pulverizing 10 mesh sieves, mixing) of same lot number respectively, place extraction kettle, add 95% ethanol (mass ratio of medical material and entrainer is 1: 1), under 40 ℃ of extraction temperature, respectively with different pressure static extracting 2h.Carried out dynamic extraction again 2 hours, and investigated the Rhizoma et radix valerianae extract yield, make the graph of relation between extracting pressure and the Rhizoma et radix valerianae extract yield,, get Rhizoma et radix valerianae extract the entrainer decompression and solvent recovery in the extract.See Fig. 1.
Experimental result shows that under uniform temp when extracting pressure increased, extract yield increased.Yield was 6.64% when extracting pressure was 30Mpa, when extracting pressure is increased to 40Mpa, and yield 6.80%.As seen when extracting pressure during greater than 30Mpa, along with pressure increases, the amplitude that yield increases is very little.Therefore obvious reduction equipment of the reduction meeting of pressure and operating cost are considered from economics point, determine that suitable extracting pressure is 30Mpa.
(2) influence of extraction temperature
Get the Rhizoma et radix valerianae coarse powder (all pulverizing 10 mesh sieves, mixing) of same lot number respectively, place extraction kettle, add 95% ethanol (mass ratio of medical material and entrainer is 1: 1), under the 30MPa extraction temperature, respectively with different temperature static extracting 2h.Dynamic extraction is 2 hours again.Investigate the Rhizoma et radix valerianae extract yield, make the graph of relation between extraction temperature and the Rhizoma et radix valerianae extract yield,, get Rhizoma et radix valerianae extract the entrainer decompression and solvent recovery in the extract.See Fig. 2.
Experimental result shows that temperature is the trend that raises and afterwards reduce earlier to the influence of extract yield.Reason is that extraction temperature is subjected to the restriction of two aspect factors to the influence of extract dissolubility: the extraction temperature sound pitch increases the solute vapour pressure on the one hand, thereby helps improving its diffusivity, helps dissolubility and increases; Extraction temperature raises and causes the shooting flow body density to reduce on the other hand, thereby has weakened fluidic extracting power, and dissolubility is reduced.The dissolubility of solute in supercritical fluid makes this result that factor is vied each other aspect two.The temperature clump is elevated to 50 ℃ for 30 ℃, and the increase of solute vapour pressure plays a major role, and extract yield is improved.But when temperature when 50 ℃ are elevated to 80 ℃, the density of supercritical fluid reduces occupies an leading position, the dissolubility of solute reduces, and extract yield is reduced.
Extract yield is approaching under 40 ℃ and the 50 ℃ of conditions, owing to consider effective proposition of heat-sensitive substance in the effective ingredient, the temperature that experiment is adopted is lower, gets 40 ℃.
(3) the entrainer consumption is investigated
Under 40 ℃ of extraction temperature, extracting pressure 30Mpa, static extracting 2h condition, investigate of the influence of the different quality proportioning (1: 0.5,1: 0.75,1: 1,1: 1.25,1: 1.5) of medical material and entrainer to extract yield.See accompanying drawing 3
As seen from Figure 3, along with the increase of entrainer ratio, the dissolubility of extract in supercritical carbon dioxide significantly improves, therefore extract yield is in rising trend, increase comparatively fast less than 1: 1.25 o'clock at mass ratio, when mass ratio equaled 1: 1.25, extract yield was 7.12%.Continue to increase the ratio of entrainer, extract yield does not have obvious raising, and quantity of solvent increases in the excessive extracting solution of entrainer, thereby has increased the workload of solvent recovery.Thereby definite entrainer consumption is 1.25 times of medical material.
In sum, the static suitable pressure that adds entrainer method extraction Rhizoma et radix valerianae is 30Mpa, and temperature is 40 ℃, and adding entrainer is 1.25: 1 with the quality of medicinal material ratio, and the static immersing time is 2h.
2 dynamically add the entrainer method
(1) selection of entrainer consumption
The addition of entrainer is wanted suitably not have effect very little, can change extraction character again too much, makes extraction mainly carry out under liquid state rather than supercriticality, causes extraction efficiency to descend.This experiment has been investigated the influence of the consumption of entrainer when being entrainer with 95% ethanol to extract yield under the condition of 40 ℃ of extraction temperature, extracting pressure 30Mpa.See Table 3.
Table 3 dynamically adds the selection of entrainer method entrainer consumption
| Entrainer accounts for the mass percent (%) of carbon dioxide | Extract yield (%) |
| 5 | 5.43 |
| 10 | 7.81 |
| 15 | 8.06 |
| 20 | 8.21 |
By table 3 as seen, the mass percent that the entrainer consumption accounts for carbon dioxide is in 5～20% scopes the time, and extract yield increases along with the increase of carrying dosage secretly, but the increase degree in the early stage clearly, then gradually is smooth trend finally.When the entrainer consumption account for carbon dioxide 10% the time, extract yield is 7.81%; And when the entrainer consumption increase to carbon dioxide 15% the time, extract yield is 8.06%, extract yield is 8.06%, increase seldom, the consumption of considering entrainer is excessive, the workload that reclaims solvent in the extract increases, and the solvent cost increase, is 10% of carbon dioxide consumption so we get the entrainer consumption.
(2) influence of extracting pressure
Get the Rhizoma et radix valerianae coarse powder (all pulverizing 10 mesh sieves, mixing) of same lot number respectively, place extraction kettle, under 40 ℃ of extraction temperature, feed CO
295% ethanol of flow 10% extracts 2h with different pressure respectively.Investigate the Rhizoma et radix valerianae extract yield, make the graph of relation between extracting pressure and the Rhizoma et radix valerianae extract yield,, get Rhizoma et radix valerianae extract the entrainer decompression and solvent recovery in the extract.See accompanying drawing 4
As seen from Figure 4: under uniform temp, when extracting pressure increased, extract yield increased.Yield was 6.85% when extracting pressure was 25Mpa, and when extracting pressure was increased to 30Mpa, yield improved little.As seen when extracting pressure during greater than 30Mpa, the amplitude that yield increases is very little.Take all factors into consideration, get 25MPa for dynamically adding the pressure of entrainer method extraction.
(3) influence of extraction temperature
Get the Rhizoma et radix valerianae coarse powder (all pulverizing 10 mesh sieves, mixing) of same lot number respectively, place extraction kettle, under the 30MPa extraction temperature, feed CO
295% ethanol of flow 10% extracts 2h with different temperature respectively.Investigate the Rhizoma et radix valerianae extract yield, make the graph of relation between extraction temperature and the Rhizoma et radix valerianae extract yield,, get Rhizoma et radix valerianae extract the entrainer decompression and solvent recovery in the extract.See accompanying drawing 5.
Extraction ratio improves along with the rising of extraction temperature as seen from Figure 5, can think that this moment, the increase of solute vapour pressure played a major role, and makes the dissolubility of extraction ratio increase thereupon.But after temperature surpassed 40 ℃, along with the increase of temperature, the amplitude that extraction ratio increases diminished, owing to consider effective proposition of heat-sensitive substance in the effective ingredient, the temperature that experiment is adopted is lower, gets 40 ℃.
In sum, the suitable pressure that dynamically adds entrainer method extraction Rhizoma et radix valerianae is 25Mpa, and temperature is 40 ℃, and the entrainer consumption is 10% of a carbon dioxide consumption.
3 use static and dynamic entrainer method simultaneously
More than two kinds of different entrainer adding modes compare, use that the required pressure of static entrainer supercritical extraction process is higher, the production cycle is longer, and use the required entrainer consumption of dynamic entrainer supercritical extraction process big.Two kinds of technology gained extraction ratios are suitable substantially.Therefore, consider two kinds of modes of carrying secretly are combined, promptly in a technology, use static and dynamic entrainer simultaneously, investigate it and can when reducing dynamic entrainer consumption, shortening the extraction time, further improve extraction ratio.
(1) the dynamically influence of entrainer consumption
Get the Rhizoma et radix valerianae coarse powder of same lot number respectively and (all pulverized 10 mesh sieves, mixing), place extraction kettle, add 95% ethanol (medical material and 95% alcoholic acid mass ratio are 1: 1.25), carry out static extracting 2h with 25Mpa, 40 ℃ of conditions, 2.5%, 5%, 10% 95% ethanol that dynamically adds carbon dioxide more respectively carries out dynamic extraction 2h, investigates extraction ratio.
The consumption of considering dynamic entrainer after being association of activity and inertia can reduce, and investigates 2.5%, 5%, 10% so dynamically add the amount of entrainer.Extraction ratio is with the Changing Pattern such as the accompanying drawing 6 of dynamic entrainer consumption.
As seen from the figure, curve presents the trend that earlier rises and afterwards become mild, is the saving cost, gets dynamic entrainer consumption and accounts for 5% of carbon dioxide and be advisable.
(2) the static immersing time is to the influence of extraction ratio
Get the Rhizoma et radix valerianae coarse powder (all pulverizing 10 mesh sieves, mixing) of same lot number, place extraction kettle, each adds 95% ethanol (medical material and 95% alcoholic acid mass ratio are 1: 1.25), respectively with 25Mpa, 40 ℃ of condition static extractings 30,60,90,120min.Feed 5% 95% alcohol extraction 2h of carbon dioxide quality then, extracting pressure is.Investigate extraction ratio.Its Changing Pattern such as Fig. 7.
Though it is few that the technology of using static entrainer and the technology of using dynamic entrainer are compared the entrainer consumption, the extraction time is longer, and unsuitable continuous production.Use static and dynamic entrainer then can when reducing dynamic entrainer consumption, shorten the extraction time effectively simultaneously.Suitable dynamic entrainer consumption, extraction temperature, extracting pressure and the static entrainer of determining in experiment and raw materials quality be than under the condition, and the selected respectively static immersing time is 30,60,90min, 2h, and the investigation static immersing time is to the influence of extraction ratio.As seen from Figure 7, curve presents the trend that rises and afterwards become mild earlier, for saving time, gets static immersing time 60min and is advisable.
Description of drawings:
Fig. 1: the static influence of adding entrainer method extracting pressure to the Rhizoma et radix valerianae extract yield
Fig. 2: the static influence of adding entrainer method extraction temperature to the Rhizoma et radix valerianae extract yield
Fig. 3: the static influence of adding entrainer method entrainer consumption to extract yield
Fig. 4: dynamically add of the influence of entrainer method extracting pressure to extraction ratio
Fig. 5: dynamically add of the influence of entrainer method extraction temperature to extraction ratio
Fig. 6: use of the influence of static and dynamic entrainer method entrainer consumption simultaneously to extraction ratio
Fig. 7: use of the influence of static and dynamic entrainer method static immersing time simultaneously to extraction ratio
The specific embodiment
Embodiment 1: the preparation of Rhizoma et radix valerianae extract
2kg is ground into coarse powder with the valerian Rhizoma et radix valerianae, crosses 10 mesh sieves, places extraction kettle, adds 95% ethanol of 2.5kg, carries out static extracting 2 hours with 30Mpa, 40 ℃ of conditions; Dynamic extraction 2h again is dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract 140g the ethanol reclaim under reduced pressure in the extract.
Embodiment 2: the preparation of Rhizoma et radix valerianae extract
2kg is ground into coarse powder with the valerian Rhizoma et radix valerianae, crosses 10 mesh sieves, places extraction kettle to extract, extracting pressure is 25Mpa, and 40 ℃ of extraction temperature are to wherein adding entrainer ethanol (account for by mass percentage carbon dioxide 10%), extraction time 2h is dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract 100g the ethanol reclaim under reduced pressure in the extract.
Embodiment 3: the preparation of Rhizoma et radix valerianae extract
2kg is ground into coarse powder with the valerian Rhizoma et radix valerianae, cross 10 mesh sieves, place extraction kettle, add the 2.5L ethyl acetate, carry out static extracting 1h with 25Mpa, 40 ℃ of conditions, dynamically add entrainer again, this moment, entrainer was ethyl acetate (accounts for by mass percentage carbon dioxide 5%), under identical extracting pressure and temperature conditions, extract 2h, be dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract 120g the ethyl acetate reclaim under reduced pressure in the extract.
Embodiment 4: tablet
Get Rhizoma et radix valerianae extract 2Kg among the embodiment 1, add adjuvant by conventional method pharmaceutically and be prepared into tablet.
Embodiment 5: granule
Get Rhizoma et radix valerianae extract 4Kg among the embodiment 2, add adjuvant by conventional method pharmaceutically and be prepared into an agent agent.
Embodiment 6: injection
Get Rhizoma et radix valerianae extract 3Kg among the embodiment 3, add adjuvant by conventional method pharmaceutically and be prepared into injection.
Embodiment 7: injectable powder
Get Rhizoma et radix valerianae extract 5Kg among the embodiment 1, add adjuvant by conventional method pharmaceutically and be prepared into injectable powder.
Embodiment 8: drop pill
Get Rhizoma et radix valerianae extract 6Kg among the embodiment 2, add adjuvant by conventional method pharmaceutically and be prepared into drop pill.
Embodiment 9: fat milk injection
Get Rhizoma et radix valerianae extract 10Kg among the embodiment 3, add adjuvant by conventional method pharmaceutically and be prepared into fat milk injection.
Embodiment 10: oral liquid
Get Rhizoma et radix valerianae extract 8Kg among the embodiment 1, add adjuvant by conventional method pharmaceutically and be prepared into oral liquid.
Embodiment 11: capsule
Get Rhizoma et radix valerianae extract 9Kg among the embodiment 2, add adjuvant by conventional method pharmaceutically and be prepared into capsule.
Claims (6)
1. Rhizoma et radix valerianae extract is characterized in that this extract is prepared from one of by the following method:
The static Ethanol Method of adding: with any coarse powder that is ground in the valerian, cross 10 mesh sieves, place extraction kettle, add ethanol, medical material and alcoholic acid mass ratio are 1: 1.25, carry out static extracting 2 hours with 30Mpa, 40 ℃ of conditions; Carry out dynamic extraction 2h again, be dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the ethanol decompression and solvent recovery in the extract;
Dynamically add Ethanol Method: any coarse powder that is ground in the valerian, cross 10 mesh sieves, place extraction kettle to extract, extracting pressure is 25Mpa, 40 ℃ of extraction temperature, be 10% of carbon dioxide by mass percentage to wherein adding alcoholic acid amount, extract time 2h, be dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the ethanol decompression and solvent recovery in the extract;
Static and dynamically add Ethanol Method: with any coarse powder that is ground in the valerian, cross 10 mesh sieves, place extraction kettle, add ethanol, medical material and alcoholic acid mass ratio are 1: 1.25, and elder generation carried out static extracting 1 hour with 25Mpa, 40 ℃; Dynamically add ethanol again, this moment, alcoholic acid amount was 5% of carbon dioxide by mass percentage, extracted 2h under identical extracting pressure and temperature conditions, was dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the ethanol decompression and solvent recovery in the extract.
2. Rhizoma et radix valerianae extract as claimed in claim 1 is characterized in that described valerian is meant all plants that contain valerian naphtha and general valerianin.
3. Rhizoma et radix valerianae extract as claimed in claim 1, it is characterized in that adding conventional adjuvant by practice of pharmacy, with Rhizoma et radix valerianae extract is that active component is made single preparations of ephedrine, or makes the medicine composition that contains the said extracted thing: tablet, soft capsule, oral liquid, drop pill, microcapsule, granule, injection, injectable powder, infusion solution or fat milk injection.
4. the extracting method of a Rhizoma et radix valerianae extract is characterized in that this method is any one in the following method:
The static Ethanol Method of adding: with any coarse powder that is ground in the valerian, cross 10 mesh sieves, place extraction kettle, add ethanol, medical material and alcoholic acid mass ratio are 1: 1.25, carry out static extracting 2 hours with 30Mpa, 40 ℃ of conditions; Carry out dynamic extraction 2h again, be dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the ethanol decompression and solvent recovery in the extract;
Dynamically add Ethanol Method: any coarse powder that is ground in the valerian, cross 10 mesh sieves, place extraction kettle to extract, extracting pressure is 25Mpa, 40 ℃ of extraction temperature, be 10% of carbon dioxide by mass percentage to wherein adding alcoholic acid amount, extract time 2h, be dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the ethanol decompression and solvent recovery in the extract;
Static and dynamically add Ethanol Method: with any coarse powder that is ground in the valerian, cross 10 mesh sieves, place extraction kettle, add ethanol, medical material and alcoholic acid mass ratio are 1: 1.25, and elder generation carried out static extracting 1 hour with 25Mpa, 40 ℃; Dynamically add ethanol again, this moment, alcoholic acid amount was 5% of carbon dioxide by mass percentage, extracted 2h under identical extracting pressure and temperature conditions, was dissolved with the supercritical CO of extract
2Enter and resolve separation in the separating still,, get Rhizoma et radix valerianae extract the ethanol decompression and solvent recovery in the extract.
5. as the extracting method of Rhizoma et radix valerianae extract as described in the claim 4, it is characterized in that described valerian is meant all plants that contain valerian naphtha and general valerianin.
6. Rhizoma et radix valerianae extract as claimed in claim 1 has the medicine of sedation or the application in the health food in preparation.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101754415A CN101396381B (en) | 2007-09-29 | 2007-09-29 | Valerian extract and preparation method and use thereof |
| HK09106560.8A HK1126982A1 (en) | 2007-09-29 | 2009-07-17 | A valerian extract and its preparative method and use |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101754415A CN101396381B (en) | 2007-09-29 | 2007-09-29 | Valerian extract and preparation method and use thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101396381A CN101396381A (en) | 2009-04-01 |
| CN101396381B true CN101396381B (en) | 2011-09-07 |
Family
ID=40515381
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101754415A Expired - Fee Related CN101396381B (en) | 2007-09-29 | 2007-09-29 | Valerian extract and preparation method and use thereof |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN101396381B (en) |
| HK (1) | HK1126982A1 (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660379B (en) * | 2012-05-03 | 2013-04-24 | 剑河县天然植物油技术开发有限公司 | Method for extracting valerian vegetable oil |
| EP3288534B1 (en) * | 2015-04-28 | 2020-09-23 | Symrise AG | Compositions comprising valerian extracts |
| CN105112296B (en) * | 2015-07-29 | 2018-07-06 | 中南林业科技大学 | One plant of angle load bacteria strain and its application in valepotriate, calming soporific class Chinese patent drug is prepared |
| CN105670784B (en) * | 2016-03-02 | 2020-01-03 | 塔里木大学 | Extraction and purification method of jujube kernel volatile oil |
| CN105687368B (en) * | 2016-03-02 | 2020-02-14 | 塔里木大学 | Application of jujube kernel volatile oil in mouse hair growth |
| CN105670798B (en) * | 2016-03-02 | 2020-01-03 | 塔里木大学 | Extraction method of jujube kernel volatile oil |
| CN106281708A (en) * | 2016-08-28 | 2017-01-04 | 广西灏源盛世生物科技有限公司 | A kind of extracting method of Rhizoma et radix valerianae quintessence oil |
| CN106490675B (en) * | 2017-01-04 | 2017-10-03 | 湖北中烟工业有限责任公司 | A kind of preparation method and applications of recombination tobacco leaf additive |
| CN107897355A (en) * | 2017-12-15 | 2018-04-13 | 柳州飞升鹏科技有限公司 | A kind of preparation method of fruit antistaling agent |
| CN113142344A (en) * | 2021-05-18 | 2021-07-23 | 北京晚安科技有限责任公司 | Sleep-aiding solid beverage and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1475490A (en) * | 2003-07-31 | 2004-02-18 | 凯 曹 | Valerian extract and its preparation method and use |
| CN1857337A (en) * | 2005-04-29 | 2006-11-08 | 肖丹 | Use of patrinia herb and its extract in preparing medicine for treating prostatic hyperplasia |
-
2007
- 2007-09-29 CN CN2007101754415A patent/CN101396381B/en not_active Expired - Fee Related
-
2009
- 2009-07-17 HK HK09106560.8A patent/HK1126982A1/en not_active IP Right Cessation
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1475490A (en) * | 2003-07-31 | 2004-02-18 | 凯 曹 | Valerian extract and its preparation method and use |
| CN1857337A (en) * | 2005-04-29 | 2006-11-08 | 肖丹 | Use of patrinia herb and its extract in preparing medicine for treating prostatic hyperplasia |
Non-Patent Citations (6)
| Title |
|---|
| 徐红.缬草挥发油对中枢神经系统药理作用的研究.《药物分析杂志》.1997,第17卷(第6期),399. * |
| 李淑芬.使用夹带剂的超临界CO2萃取.《高等制药分离工程》.2004,91-93. * |
| 李迎春等.超临界流体萃取中草药的研究进展.《广州化学》.2000,第25卷(第03期),59-63. * |
| 杨海燕.超临界CO2流体萃取缬草精油的研究.《新疆农业大学学报》.1998,第21卷(第1期),43-46. * |
| 金竹萍.超临界流体萃取技术的应用及研究进展.《山西化工》.2007,第27卷(第02期),42-45. * |
| 黄宝康.国产缬草属药用植物资源调查.《中药材》.2004,第27卷(第9期),632-634. * |
Also Published As
| Publication number | Publication date |
|---|---|
| HK1126982A1 (en) | 2009-09-18 |
| CN101396381A (en) | 2009-04-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101396381B (en) | Valerian extract and preparation method and use thereof | |
| RU2395293C2 (en) | Pharmaceutical composition for treatment of depression and method of obtaining it | |
| CN101161324B (en) | Sub-critical fluid extraction solvent and abstraction method | |
| CN107865890B (en) | Slug extract, extraction and separation method of effective components in extract and application | |
| CN103040882B (en) | Passiflora edulis sims stem-leaf extract as well as pharmaceutical composition and antidepressant action of extract | |
| CN1895353B (en) | Preparation of compound Danshen tablets | |
| CN102114060B (en) | Amur valeriana extract and preparation method and applications thereof | |
| BRPI0722181A2 (en) | "ANTIMELANCOLIC MEDICINAL PRODUCT PREPARED WITH JUJUBA CAMP-BASED MATERIALS" | |
| CN104387362B (en) | A kind of iridoidate compound, its preparation method and application | |
| WO2013155995A1 (en) | Red yeast and kudzu root pharmaceutical composition for regulating blood lipids and preparation method therefor | |
| CN102641324A (en) | Herba gueldenstaedtia extract and uses thereof | |
| CN102178721B (en) | Application of fiveleaf gynostemma herb suspension and extract to preparation of drug for treating and resisting depression | |
| CN101371858A (en) | Patrinia scaniosaefolia extract as well as preparation method and application thereof | |
| CN100477996C (en) | Extract of star of bethlehem and its prepn process, medicinal composition and use | |
| CN104804056A (en) | Sarcopyramis nepalensis extract and application thereof | |
| CN103816210A (en) | Pueraria lobata extract and application thereof | |
| CN109939100B (en) | Acetylcholine enzyme inhibitor prepared from Cyrtomium fortunei, preparation method and application | |
| CN101375983B (en) | Chinese medicinal composition for treating dysmenorrhea and preparation method thereof | |
| CN107854519A (en) | A kind of perilla leaf oil and its application | |
| AU2020100748A4 (en) | Preparation method and application of alkaloids from cynanchum komarovii | |
| CN100363018C (en) | Honeysuckle flower soft capsule and preparation method thereof | |
| CN104644992B (en) | The Chinese medicine composition and preparation method of a kind of nourishing blood and tranquilization | |
| CN109820883A (en) | Metapanax plant extracts and its pharmaceutical composition preparation method and its antiulcer purposes | |
| CN109908120B (en) | Effective component of Dryopteris stenoptera, extraction method and application thereof | |
| CN102048860A (en) | Nasosinusitis soft capsule pharmaceutical preparation and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| REG | Reference to a national code |
Ref country code: HK Ref legal event code: DE Ref document number: 1126982 Country of ref document: HK |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| REG | Reference to a national code |
Ref country code: HK Ref legal event code: GR Ref document number: 1126982 Country of ref document: HK |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110907 Termination date: 20150929 |
|
| EXPY | Termination of patent right or utility model |