CN103623250A - Preparation technology of active freeze-dried rhizoma gastrodiae - Google Patents
Preparation technology of active freeze-dried rhizoma gastrodiae Download PDFInfo
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- CN103623250A CN103623250A CN201310667256.3A CN201310667256A CN103623250A CN 103623250 A CN103623250 A CN 103623250A CN 201310667256 A CN201310667256 A CN 201310667256A CN 103623250 A CN103623250 A CN 103623250A
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- freeze
- rhizoma gastrodiae
- drying
- gastrodia elata
- dried
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000005516 engineering process Methods 0.000 title claims abstract description 16
- 238000004108 freeze drying Methods 0.000 claims abstract description 52
- PUQSUZTXKPLAPR-UJPOAAIJSA-N Gastrodin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=C(CO)C=C1 PUQSUZTXKPLAPR-UJPOAAIJSA-N 0.000 claims abstract description 16
- PUQSUZTXKPLAPR-KSSYENDESA-N 4-(beta-D-Glucopyranosyloxy) benzyl alcohol Natural products O([C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1)c1ccc(CO)cc1 PUQSUZTXKPLAPR-KSSYENDESA-N 0.000 claims abstract description 9
- 229930193974 gastrodin Natural products 0.000 claims abstract description 9
- PUQSUZTXKPLAPR-NZEXEKPDSA-N helicidol Natural products O([C@H]1[C@H](O)[C@H](O)[C@@H](O)[C@@H](CO)O1)c1ccc(CO)cc1 PUQSUZTXKPLAPR-NZEXEKPDSA-N 0.000 claims abstract description 9
- 241000305491 Gastrodia elata Species 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 229920000742 Cotton Polymers 0.000 claims description 7
- 210000000589 cicatrix Anatomy 0.000 claims description 4
- 239000002671 adjuvant Substances 0.000 claims description 2
- 230000000295 complement effect Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 239000008194 pharmaceutical composition Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000011160 research Methods 0.000 abstract description 2
- 230000000717 retained effect Effects 0.000 abstract description 2
- 231100000241 scar Toxicity 0.000 abstract 1
- 238000007790 scraping Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 6
- 238000009835 boiling Methods 0.000 description 2
- 239000007910 chewable tablet Substances 0.000 description 2
- 229940068682 chewable tablet Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 206010010904 Convulsion Diseases 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 241000233855 Orchidaceae Species 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 206010043376 Tetanus Diseases 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000036461 convulsion Effects 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 206010015037 epilepsy Diseases 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000002496 gastric effect Effects 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 210000002435 tendon Anatomy 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009777 vacuum freeze-drying Methods 0.000 description 1
- 238000009461 vacuum packaging Methods 0.000 description 1
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a preparation technology of active freeze-dried rhizoma gastrodiae, which comprises the following operations of cleaning fresh rhizoma gastrodiae, scraping the coarse cortex and scar of fresh rhizoma gastrodiae, slicing and freeze-drying fresh rhizoma gastrodiae, wherein the freeze-drying operation is that rhizoma gastrodiae slices formed after rhizoma gastrodiae is sliced are put in a freeze dryer, and are vacuumized till the vacuum degree is 12-15 Pa after being cooled to -45 to -55 DEG C, the temperature is held, and the freeze-drying is carried out for 40-48 h under the pressure, so that the rhizoma gastrodiae freeze-dried slices are obtained. The invention further provides freeze-dried rhizoma gastrodiae prepared by the preparation technology. Researches find that fresh rhizoma gastrodiae is directly freeze-dried under the technological condition, so that the content of gastrodin can be retained effectively, good freeze-dried product appearance and shape are ensured, and the possibility of late hot sell of the rhizoma gastrodiae freeze dried slices is provided; meanwhile, on the premise of meeting the appearance and the product quality, the technology can reach the optimal freeze-drying rate, saves the freeze-drying time effectively, and facilitates saving of the production cost.
Description
Technical field
The present invention relates to the preparation technology of the dry Rhizoma Gastrodiae of a kind of active ice.
Background technology
Rhizoma Gastrodiae, is the tuber of orchid Rhizoma Gastrodiae, is to commonly use and famousr and precious Chinese medicine simply, the disease such as clinical dizzy, the numb limbs and tense tendons of being used for having a headache, infantile convulsion, epilepsy, tic, tetanus, and its main active is gastrodine.
Traditional Rhizoma Gastrodiae processing procedure is after adopting steaming method or cooking method to process, then dries or dry.Yet the researchs such as Yong Wu show, in conventional processes, the active component of Rhizoma Gastrodiae can a large amount of losses, as gastrodine.The disclosed lyophilizing mode of the document is: by Rhizoma Gastrodiae by lyophilization, can improve gastrodin content, its freezing method is as follows: in vacuum freeze drier cryodesiccation chamber, shelf temperature is down to-20 ℃, again Rhizoma Gastrodiae is put on the shelf of freeze drying box, after 1h, shelf temperature reaches-40 ℃, and products temperature is-22 ℃.Open vacuum pump, pressure is evacuated to 30～60Pa left and right, and freeze drying box stops refrigeration, and water vapour coagulator continues refrigeration; Cross after 1h, freeze drying box shelf is heated, controller firing rate, until shelf temperature and sample temperature while being close, stop heating, takes out sample, vacuum packaging, and whole freeze-drying process lasts 12h left and right.This freeze drying process, can retain gastrodin content, and surface white, give off a strong fragrance loose, and the large and porous in gap, section white (Yong Wu, etc., the comparative study of different dry drying method to Rhizoma Gastrodiae quality influence, Chinese patent medicine, 27 6 phases of volume in 2005).Number of patent application: 201210518584.2, a kind of preparation method of freeze-drying gastrodia elata chewable tablet is disclosed, it is that Rhizoma Gastrodiae is boiling hot by boiling, cooling, section, after cleaning color fixative, carry out frozen dried, step of freeze drying is: first Rhizoma Gastrodiae slice is placed at-35 ℃ and freezes, the cold well temperature of freeze dryer drops to below-40 ℃, then the Rhizoma Gastrodiae slice having freezed is put into dry vacuum container, evacuation, at pressure, be under 40～60Pa, to freeze 1 hour, dry 24～25 hours of resublime, after sublimation drying, carry out again the parsing-desiccation of 3～5 hours, when in storehouse to be dried, pressure is 20～30Pa, deliver from godown, obtain moisture and be 2～5% freeze-drying gastrodia elata chewable tablet.
Discovery when inventor adopts prior art to carry out lyophilizing to Rhizoma Gastrodiae slice, although adopt existing freeze-dry process can reduce gastrodine loss, yet the Rhizoma Gastrodiae slice after lyophilizing can be out of shape or sliver, can not more intactly keep raw product original state, the later stage that has a strong impact on freeze-drying gastrodia elata sheet sells.In addition, in some method, before lyophilizing, also Rhizoma Gastrodiae is boiled to scald and kill enzyme, due to the existence of hot conditions, also increased the loss amount of gastrodine.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology that gastrodin content can effectively be retained and maintain the dry Rhizoma Gastrodiae of active ice of day Taro Aso's product original state.
The invention provides the preparation technology of the dry Rhizoma Gastrodiae of a kind of active ice, the preparation technology of the dry Rhizoma Gastrodiae of active ice, it comprises cleans, goes rough bark and cicatrix, section and lyophilizing operation sequence to fresh gastrodia elata, described lyophilizing operation is as follows: the Rhizoma Gastrodiae slice after section is placed in to freezer dryer, be cooled to after-45～-55 ℃, being evacuated to vacuum is 12～15Pa again, keep said temperature and pressure lyophilizing 40～48 hours, obtain Rhizoma Gastrodiae lyophilizing sheet (this Rhizoma Gastrodiae lyophilizing sheet also can be described as the dry Rhizoma Gastrodiae of active ice).
Further, described freeze-drying time is 48 hours.Under this freeze-drying time, can guarantee that freeze-drying gastrodia elata sheet obtains water content in 2.0%, be more conducive to the stability of freeze-drying gastrodia elata sheet in storage process.
Further, the thickness of Rhizoma Gastrodiae section is 1cm ± 0.2cm.As everyone knows, in dry run, the thickness of pharmaceutical decocting piece also has certain influence to the rate of volatilization of moisture, and for the present invention, all with Rhizoma Gastrodiae slice thickness have certain associated with water content the drying time of Rhizoma Gastrodiae lyophilizing sheet.
Further, after Rhizoma Gastrodiae section, first Rhizoma Gastrodiae slice is tied up with cotton thread, then carried out lyophilizing.Cotton thread is tied up after lyophilizing, and the outward appearance of dried frozen aquatic products, shape size and raw product Rhizoma Gastrodiae integral body are very approximate, and select the reason of cotton thread to be herein, and cotton thread still keeps soft quality under cryogenic conditions, can not cause damage to Rhizoma Gastrodiae dried frozen aquatic products outward appearance.Certainly, in concrete freeze-drying process, also can after lyophilizing, then tie up without tying up, also the outward appearance of reducible whole Rhizoma Gastrodiae and shape size.
The freeze-drying gastrodia elata that the present invention also provides above-mentioned technique to prepare.
Wherein, in described freeze-drying gastrodia elata, gastrodin content is 0.5～1.0%, and water content is in 5.0%.
Further, in described freeze-drying gastrodia elata, water content is in 2.0%.
The present invention also provides a kind of pharmaceutical composition, and it is the medicated powder with above-mentioned freeze-drying gastrodia elata, or the water of freeze-drying gastrodia elata or extractive with organic solvent be active component, adds the preparation that pharmaceutically conventional adjuvant or complementary composition are prepared from.
Described preparation can be gastrointestinal administration preparation, Percutaneously administrable preparation or injection etc.
The present invention studies discovery, by fresh gastrodia elata directly lyophilizing under process conditions of the present invention, can effectively retain gastrodin content, guarantees good dried frozen aquatic products face shaping, for the later stage fast sale of Rhizoma Gastrodiae lyophilizing sheet provides may; , meeting under the prerequisite of outward appearance and product quality, technique of the present invention has also reached best freeze drying rate, has effectively saved freeze-drying time, is conducive to the saving of production cost meanwhile.
Accompanying drawing explanation
Dried frozen aquatic products photo prepared by Fig. 1 technique of the present invention;
The photo of freeze-drying gastrodia elata sheet when Fig. 2 vacuum is greater than 15Pa;
The photo of freeze-drying gastrodia elata sheet when Fig. 3 vacuum is greater than 15Pa;
The photo of Fig. 4 vacuum freeze-drying gastrodia elata sheet when 12～15Pa;
By Fig. 2,3, can be found out, when vacuum is greater than 15Pa, freeze-drying gastrodia elata sheet has the phenomenons such as crackle, fold and flexural deformation; As seen from Figure 4, freeze-drying gastrodia elata sheet surfacing prepared by the inventive method, corrugationless distortion and sliver phenomenon.
The specific embodiment
In the present invention, gastrodine and moisture all detect according to < < Chinese Pharmacopoeia > 2010 editions Firsts of > " Rhizoma Gastrodiae " lower regulation.The freezer dryer using in the present invention is bought from Beijing development in science and technology company limited of Song Yuan Huaxing, and model is GZLY-5.
Embodiment 1
Get fresh gastrodia elata, clean, go, after rough bark and cicatrix, to be cut into the thin slice of 1 ± 0.2cm, after Rhizoma Gastrodiae slice is tied up with cotton thread, be placed in freezer dryer, be first cooled to after-45～-55 ℃, open vacuum pump, being evacuated to vacuum is 12～15Pa, keeps said temperature and Vacuum Pressure lyophilizing 48 hours, takes out, obtain Rhizoma Gastrodiae lyophilizing sheet, as seen from Figure 1, the dry Rhizoma Gastrodiae of active ice prepared by the present invention, its shape size and outward appearance and raw product Rhizoma Gastrodiae be zero difference almost.
Embodiment 2
Get fresh gastrodia elata, clean, go after rough bark and cicatrix, be cut into the thin slice of 1 ± 0.2cm, after Rhizoma Gastrodiae slice is tied up with cotton thread, be placed in freezer dryer, first be cooled to after-45～-55 ℃, open vacuum pump, being evacuated to vacuum is 12～15Pa, keeps said temperature and Vacuum Pressure lyophilizing 40 hours, take out, obtain Rhizoma Gastrodiae lyophilizing sheet.
Get 10 batches of fresh gastrodia elatas, selected shape, the Rhizoma Gastrodiae individuality that weight is approximate, process according to the method for embodiment 1,2 respectively, and measure gastrodine and moisture, the results are shown in following table:
| ? | Gastrodine (%) | Moisture (%) |
| Embodiment 1 | 0.5～1.0 | In 2.0 |
| Embodiment 2 | 0.5～1.0 | Be greater than 2.0 and be less than or equal to 5.0 |
From said determination result, in freeze-drying gastrodia elata sheet prepared by the freeze-dry process of embodiment 1,2, gastrodin content is all higher, and moisture all meets decoction pieces standard.Further relatively find, under lyophilisation condition of the present invention, if lyophilizing more than 40 hours, can guarantee that dried frozen aquatic products water content remains in 5.0%, if freeze-drying time reaches 48 hours, can guarantee that water content is in 2.0%.As everyone knows, water content is lower, more can guarantee the quality stability in dried frozen aquatic products later stage storage process, and therefore, the present invention is preferably lyophilizing 48 hours finally.
Inventor finds in earlier stage; adopt existing freeze drying technology, conventionally can cause Rhizoma Gastrodiae slice change of shape or sliver, have a strong impact on product appearance; the preliminary experiment that inventor's process is nearly 2000 times, the conditions such as freeze temperature and vacuum of finally finding all have appreciable impact to product appearance and freeze drying rate:
(1) when vacuum is greater than 15Pa, although can shorten freeze-drying time, Rhizoma Gastrodiae slice shape produces obviously and changes, and even has sliver phenomenon, and increases with vacuum, and cosmetic variation is more serious, and therefore, wish is selected to carry out lyophilizing (seeing Fig. 2～4) compared with rough vacuum; Yet when vacuum is less than 12Pa, under same freeze temperature, freeze-drying time extends, need under 72 hours or longer time, could be dried at-45 ℃～-55 ℃ completely, reach 5% with interior water content.
(2) inventor surprisingly finds, freeze temperature is during lower than-55 ℃ or higher than-45 ℃ time, water sublimed speed all can obviously slow down, under identical vacuum, drying time, ratio-45 ℃～-55 ℃ increased by 30%,, under vacuum 12～15Pa condition, only have when freeze temperature is-45 ℃～-55 ℃, just can reach best freeze drying rate, effectively save freeze-drying time.
Comprehensive trial test result repeatedly, the present invention has finally determined that lyophilization temperature is-45 ℃～-55 ℃, vacuum is 12～15Pa, directly lyophilizing with this understanding, not only can effectively retain gastrodin content, guarantee good dried frozen aquatic products face shaping, also reached best freeze drying rate, effectively saved freeze-drying time.
Claims (8)
1. the preparation technology of the dry Rhizoma Gastrodiae of active ice, it comprises cleans, goes rough bark and cicatrix, section and lyophilizing operation sequence to fresh gastrodia elata, it is characterized in that: described lyophilizing operation is as follows: the Rhizoma Gastrodiae slice after section is placed in to freezer dryer, be cooled to after-45～-55 ℃, being evacuated to vacuum is 12～15Pa again, keep said temperature and pressure lyophilizing 40～48 hours, obtain Rhizoma Gastrodiae lyophilizing sheet.
2. preparation technology according to claim 1, is characterized in that: described freeze-drying time is 48 hours.
3. preparation technology according to claim 1, is characterized in that: the thickness of Rhizoma Gastrodiae section is 1cm ± 0.2cm.
4. according to the preparation technology described in claim 1 or 3, it is characterized in that: after Rhizoma Gastrodiae section, first Rhizoma Gastrodiae slice is tied up with cotton thread, then carried out lyophilizing.
5. the freeze-drying gastrodia elata that described in claim 1～4 any one prepared by technique.
6. freeze-drying gastrodia elata according to claim 5, is characterized in that: in described freeze-drying gastrodia elata, gastrodin content is 0.5～1.0%, and water content is in 5.0%.
7. freeze-drying gastrodia elata according to claim 6, is characterized in that: in described freeze-drying gastrodia elata, water content is in 2.0%.
8. a pharmaceutical composition, it is characterized in that: it is the medicated powder with freeze-drying gastrodia elata described in claim 5～7 any one, or the water of freeze-drying gastrodia elata or extractive with organic solvent be active component, add the preparation that pharmaceutically conventional adjuvant or complementary composition are prepared from.
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| CN201310667256.3A CN103623250B (en) | 2013-12-10 | 2013-12-10 | Preparation technology of active freeze-dried rhizoma gastrodiae |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310667256.3A CN103623250B (en) | 2013-12-10 | 2013-12-10 | Preparation technology of active freeze-dried rhizoma gastrodiae |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104288530A (en) * | 2014-09-19 | 2015-01-21 | 陕西科技大学 | Method for preparing gastrodia elata slices |
| CN105998744A (en) * | 2016-05-23 | 2016-10-12 | 云南威信盛宝农业科技有限公司 | Gastrodia tuber microwave/freeze drying multiplex drying processing method |
| CN107753766A (en) * | 2017-11-23 | 2018-03-06 | 昭通市骅成制药有限公司 | A kind of preparation method of Processed Product of Rhizoma Gastrodiae |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1222374A (en) * | 1998-01-09 | 1999-07-14 | *** | Active Gastrodia elata and its preparation |
| CN103005434A (en) * | 2012-12-06 | 2013-04-03 | 四川锡成天然食品有限公司 | Freeze-dried gastrodia elata chewable tablet manufacturing method |
-
2013
- 2013-12-10 CN CN201310667256.3A patent/CN103623250B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1222374A (en) * | 1998-01-09 | 1999-07-14 | *** | Active Gastrodia elata and its preparation |
| CN103005434A (en) * | 2012-12-06 | 2013-04-03 | 四川锡成天然食品有限公司 | Freeze-dried gastrodia elata chewable tablet manufacturing method |
Non-Patent Citations (1)
| Title |
|---|
| 秦俊哲等: "不同炮制方法对天麻素含量的影响", 《陕西科技大学学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104288530A (en) * | 2014-09-19 | 2015-01-21 | 陕西科技大学 | Method for preparing gastrodia elata slices |
| CN105998744A (en) * | 2016-05-23 | 2016-10-12 | 云南威信盛宝农业科技有限公司 | Gastrodia tuber microwave/freeze drying multiplex drying processing method |
| CN107753766A (en) * | 2017-11-23 | 2018-03-06 | 昭通市骅成制药有限公司 | A kind of preparation method of Processed Product of Rhizoma Gastrodiae |
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