CN101658621A - Method for preparing freeze-dried powder containing alliin and allinase - Google Patents
Method for preparing freeze-dried powder containing alliin and allinase Download PDFInfo
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- CN101658621A CN101658621A CN200810042244A CN200810042244A CN101658621A CN 101658621 A CN101658621 A CN 101658621A CN 200810042244 A CN200810042244 A CN 200810042244A CN 200810042244 A CN200810042244 A CN 200810042244A CN 101658621 A CN101658621 A CN 101658621A
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- allinase
- alliin
- powder
- dried powder
- celsius
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Abstract
The invention provides a method for preparing freeze-dried powder containing alliin and allinase acquired from fresh garlic, which is suitable for batch production, and comprises the following steps:preprocessing the fresh garlic firstly; conveying the garlic of the step 1 to a hammer mill and injecting liquid nitrogen into the hammer mill simultaneously so as to generate low temperature and enable the hardness of garlic flakes to meet the requirement of pulverization, and hammering the garlic flakes to obtain ice powder; transferring the ice powder to a balance chamber so as to equalize thetemperature of the ice powder at minus 40 DEG C; and transferring the ice powder of which the average temperature is at minus 40 DEG C to a vacuum drying device, raising the temperature gradually to reach 40 DEG C and vacuum degree of 0.5 Pa, and preparing the freeze-dried powder containing the alliin and the allinase after at least 10 hours.
Description
Technical field
The present invention relates to the preparation method of allicin precursor chemical constituent, be specifically related to a kind of preparation method that contains the lyophilized powder of alliin and allinase.
Background technology
Bulbus Allii is time-honored medicine food dual purpose plant, is the underground bulb of Liliaceae allium Bulbus Allii.Recent studies finds, that Bulbus Allii has is anticancer, blood fat reducing, kill effect such as fungus, becomes the focus of countries in the world biomedical research.
Garlicin (Allicin, diallyl thiosulfinate) is the unlimited medicinal compound of a kind of prospect.Because its chemical property is extremely unstable, extract and preserve all very big difficulty of existence.Therefore the countries in the world scientist is devoted to research and develop a kind of medicinal intermediate that contains garlicin precursor chemical analysis.Garlicin precursor chemical constituent comprises alliin, allinase.
Alliin (Alliin, 2-allyl cysteine sulfoxide) has another name called alliin, mainly is present in the cell of fresh garlic bulbil, and no color or smell, chemical property is relatively stable.
(Allinase EC4.4.1.4) has another name called alliin lyase, alkylthio cysteine enzyme to allinase, is present in the vacuole of cell.Generally acknowledge at present allinase catalysis alliin to produce serial volatility organic compounds containing sulfur such as allicin (Allicin), 4,5,9-trithiadodeca-1,6,11-triene 9-oxide. (Ajoenes) and bring into play multiple drug effect.
Alliin and allinase independently are present in respectively in the bulb of Bulbus Allii, and these two kinds of materials can be in contact with one another after bulb is smashed to pieces, and decomposition reaction takes place rapidly.So it is very difficult obtaining that a kind of alliin and allinase stably be present in the pharmaceutical intermediate among a kind of material simultaneously.
Summary of the invention
The method of from fresh garlic, obtaining the medicinal intermediate that contains garlicin precursor chemical analysis that the object of the present invention is to provide a kind of suitable batch to produce.
For reaching above-mentioned purpose, the present invention takes following technical scheme:
A kind of method for preparing freeze-dried powder that contains alliin and allinase comprises the steps:
1) at first fresh Bulbus Allii is carried out pretreatment;
2) Bulbus Allii in the step 1 is delivered in the beater grinder, the liquid nitrogen of annotating simultaneously produces low temperature immediately, makes the satisfied pulverizing of hardness of Bulbus Allii garlic clove required, obtains ice powder after the hammering;
3) above-mentioned ice powder is transferred in the balance cylinder, the temperature equalization that makes ice powder is at 40 degrees below zero Celsius;
4) be above-mentioned mean temperature that the ice powder of 40 degrees below zero Celsius is transplanted in the Minton dryer, be warming up to 40 degree Celsius gradually, vacuum is 0.5Pa, through obtaining containing the lyophilized powder of alliin and allinase after at least 10 hours.
Further, the pretreatment of described step 1 be meant the peeling of bright Bulbus Allii, be placed on after cleaning Celsius subzero 5 ℃ standby to the subzero 10 ℃ room temperature storehouse Celsius.
Be 0.7～1.5 times addition filling liquid nitrogen in the further described step 2, produce the low temperature of subzero 196 degree Celsius, cross 20 mesh sieves after the hammering and obtain ice powder according to the garlic clove volume.
Further, the time of ice powder in the balance cylinder is 1 to 3 hour in the described step 3.
Further, be 3% the lyophilized powder that contains alliin and allinase through obtaining water content in 10 to 12 hours in the described step 4.
Further, the alliin content of the last lyophilized powder that obtains restrains up to 30mg-35mg/ in the described step 4, and enzyme activity does not reduce.
The present invention's cryotherapy crushing technology makes all chemical constituent dormancy in the bright Bulbus Allii, carries out following process again under subzero 196 ℃ of temperature Celsius, the ice powder after the pulverizing carries out sublimation drying can be prepared into the lyophilized powder that contains alliin and allinase.Thereby guaranteed effectively that in whole process of preparation alliin and allinase avoid interacting and effective ingredient is transformed and run off.Realized that effective monomer exists with original shape, guaranteed drug effect performance in vivo.The prepared material of the present invention does not detect dissolvent residual as yet, and good economy performance, does not have any pollutant and produces.Whole process of preparation of the present invention guarantees that under the GMP state every sanitary index of manufactured goods is up to standard.
The specific embodiment
A kind of method for preparing freeze-dried powder that contains alliin and allinase of the present invention comprises the steps:
The first step is carried out bright Bulbus Allii pretreatment: be placed in the storehouse of subzero 5 ℃～subzero 10 ℃ of room temperatures Celsius Celsius standby with the peeling of bright Bulbus Allii, after cleaning;
Second step, the garlic clove of cleaning is delivered in the beater grinder simultaneously 0.7～1.5 times addition filling liquid nitrogen by the garlic clove volume, produce subzero 196 ℃ of low temperature Celsius immediately, it is required to make garlic clove hardness satisfy pulverizing, hammering is pulverized 100% and is crossed 20 mesh sieves, obtain ice powder, beater grinder is made by U.S. VIRTIS company.
The 3rd step was transferred in the balance cylinder 1～3 hour to ice powder, made its temperature equalization at subzero 40 ℃ Celsius.
The 4th step, is mean temperature that subzero 40 ℃ ice powder Celsius is placed the intensification of vacuum desiccator inner control from subzero 40 ℃ to 40 ℃ Celsius Celsius, vacuum is 0.5Pa, through 10～12 hours water content is 3% lyophilized powder, Minton dryer is made by Denmark ATLAS company.
Above-mentioned steps can suppress the decomposition reaction of allinase and alliin in the technical process fully, and the lyophilized powder of acquisition can guarantee the initial condition of effective monomer.
Its alliin content of the lyophilized powder of this prepared can restrain up to 30mg-35mg/, and enzyme activity can not reduce.
Adopt high performance liquid chromatograph (HPLC) to measure the garlicin of alliin, allinase reaction generation.Calculate that with alliin, the maximum release ratio of allinase every gram lyophilized powder includes the actual content of alliin and allinase at 2: 1; 0～5 minute catalytic reaction of curved demonstration presents first order reaction during its dynamic response, and reaction in 5～25 minutes presents the mixed class reaction, and 25 minutes～13 hours near zero order reaction.5 minutes was the enzymatic reaction initial velocity with in, reached maximum reaction velocity by 25 minutes.Garlicin concentration increases in time, reaches stable to 13 hour concentrations in 25 minutes.
Claims (6)
1. a method for preparing freeze-dried powder that contains alliin and allinase is characterized in that, comprises the steps:
1) at first fresh Bulbus Allii is carried out pretreatment;
2) Bulbus Allii in the step 1 is delivered in the beater grinder, the liquid nitrogen of annotating simultaneously produces low temperature immediately, makes the satisfied pulverizing of hardness of Bulbus Allii garlic clove required, obtains ice powder after the hammering;
3) above-mentioned ice powder is transferred in the balance cylinder, the temperature equalization that makes ice powder is at 40 degrees below zero Celsius;
4) be above-mentioned mean temperature that the ice powder of 40 degrees below zero Celsius is transplanted in the Minton dryer, be warming up to 40 degree Celsius gradually, vacuum is 0.5Pa, through obtaining containing the lyophilized powder of alliin and allinase after at least 10 hours.
2. a kind of method for preparing freeze-dried powder that contains alliin and allinase as claimed in claim 1 is characterized in that, the pretreatment of described step 1 is meant the peeling of bright Bulbus Allii, be placed on after cleaning Celsius subzero 5 ℃ standby to the subzero 10 ℃ room temperature storehouse Celsius.
3. a kind of method for preparing freeze-dried powder that contains alliin and allinase as claimed in claim 1, it is characterized in that, be 0.7～1.5 times addition filling liquid nitrogen in the described step 2, produce the low temperature of subzero 196 degree Celsius, cross 20 mesh sieves after the hammering and obtain ice powder according to the garlic clove volume.
4. a kind of method for preparing freeze-dried powder that contains alliin and allinase as claimed in claim 1 is characterized in that, the time of ice powder in the balance cylinder is 1 to 3 hour in the described step 3.
5. a kind of method for preparing freeze-dried powder that contains alliin and allinase as claimed in claim 1 is characterized in that, is 3% the lyophilized powder that contains alliin and allinase through obtaining water content in 10 to 12 hours in the described step 4.
6. a kind of method for preparing freeze-dried powder that contains Bulbus Allii ammonia enzyme and allinase as claimed in claim 1 is characterized in that, the alliin content of the last lyophilized powder that obtains restrains up to 30mg-35mg/ in the described step 4, and enzyme activity does not reduce.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810042244A CN101658621A (en) | 2008-08-29 | 2008-08-29 | Method for preparing freeze-dried powder containing alliin and allinase |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810042244A CN101658621A (en) | 2008-08-29 | 2008-08-29 | Method for preparing freeze-dried powder containing alliin and allinase |
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| CN101658621A true CN101658621A (en) | 2010-03-03 |
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| CN200810042244A Pending CN101658621A (en) | 2008-08-29 | 2008-08-29 | Method for preparing freeze-dried powder containing alliin and allinase |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102058878A (en) * | 2010-12-21 | 2011-05-18 | 中国药科大学 | Prosoma pellet tablet for generating allicin in stomach and preparation method thereof |
| CN102217759A (en) * | 2010-04-16 | 2011-10-19 | 乌鲁木齐宏信科创生物科技有限公司 | Production method of novel sea buckthorn all-fruit powder |
| CN108434307A (en) * | 2018-03-09 | 2018-08-24 | 新疆埃乐欣药业有限公司 | Antipruritic anti-acne garlic ointment of inhibiting bacteria and diminishing inflammation and its preparation method and application |
-
2008
- 2008-08-29 CN CN200810042244A patent/CN101658621A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102217759A (en) * | 2010-04-16 | 2011-10-19 | 乌鲁木齐宏信科创生物科技有限公司 | Production method of novel sea buckthorn all-fruit powder |
| CN102058878A (en) * | 2010-12-21 | 2011-05-18 | 中国药科大学 | Prosoma pellet tablet for generating allicin in stomach and preparation method thereof |
| CN102058878B (en) * | 2010-12-21 | 2013-04-10 | 中国药科大学 | Prosoma pellet tablet for generating allicin in stomach and preparation method thereof |
| CN108434307A (en) * | 2018-03-09 | 2018-08-24 | 新疆埃乐欣药业有限公司 | Antipruritic anti-acne garlic ointment of inhibiting bacteria and diminishing inflammation and its preparation method and application |
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Owner name: SHANGHAI FANG YUAN TECHNOLOGY DEVELOPMENT CO., LTD |
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Effective date of registration: 20100415 Address after: 200061 room 1715, No. 708, Shanghai, Zhongshan North Road Applicant after: Shanghai Jialishen Pharmaceuticals Co., Ltd. Co-applicant after: Shanghai Fangyuan Science & Technology Development Co., Ltd. Address before: 200061 room 1715, No. 708, Shanghai, Zhongshan North Road Applicant before: Shanghai Jialishen Pharmaceuticals Co., Ltd. |
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Open date: 20100303 |