CN105348334A - Method for simultaneously extracting gastrodia elata oil and gastrodin from gastrodia elata - Google Patents
Method for simultaneously extracting gastrodia elata oil and gastrodin from gastrodia elata Download PDFInfo
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- CN105348334A CN105348334A CN201510833959.8A CN201510833959A CN105348334A CN 105348334 A CN105348334 A CN 105348334A CN 201510833959 A CN201510833959 A CN 201510833959A CN 105348334 A CN105348334 A CN 105348334A
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- crude product
- gastrodine
- gastrodia elata
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/203—Monocyclic carbocyclic rings other than cyclohexane rings; Bicyclic carbocyclic ring systems
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
Abstract
The invention discloses a method for simultaneously extracting gastrodia elata oil and gastrodin from gastrodia elata. The method comprises the steps of: 1) adding crushed gastrodia elata tuber powders into a high-pressure tank, then injecting anhydrous ethanol, after uniformly mixing, carrying out circular extraction for 3-5 times at a certain pressure and temperature, collecting and extracting slurry, and filtering the slurry to obtain a filtrate A; 2) carrying out vacuum recovery on the filtrate A to obtain a gastrodia elata crude product; 3) extracting the gastrodia elata crude product by using an extracting agent, after uniformly mixing, leaving the gastrodia elata crude product to stand and layering the gastrodia elata crude product, wherein the upper layer is gastrodia elata oil and the lower layer is a gastrodin crude product A; or leaving the gastrodia elata crude product to stand and settling the gastrodia elata crude product, and collecting the precipitate to obtain a gastrodin crude product B; 4) carrying out vacuum concentration on the gastrodin crude product A and then extracting the gastrodin crude product A by using petroleum ether, or extracting the gastrodin crude product B by using petroleum ether, and carrying out concentration and drying on the lower layer aqueous phase to obtain grey powders; and 5) soaking the grey powders with petroleum ether, and then filtering and drying the grey powders to obtain gastrodin. The method disclosed by the invention is simple and feasible and can be used for simultaneously extracting gastrodia elata oil and gastrodin.
Description
Technical field
The present invention relates to Chinese medicinal materials chemical composition extractive technique field, be specifically related to a kind of method simultaneously extracting sky sesame oil and Gastrodine from rhizoma Gastrodiae, the method makes the functional component of rhizoma Gastrodiae and medicinal ingredients be fully used.
Background technology
Rhizoma Gastrodiae is the orchid family Gastrodia perennial herb phytoparasite, has plump root stock, its root stock be used as medicine to have a dizzy spell in order to treatment, the illness such as numb limbs and tense tendons and infantile convulsion, be rare Chinese medicine, share to be used for the treatment of with the precious glossy ganoderma of fine jade and have a headache, have a sleepless night.The primary medicinal component of Gastrodia Elata Stem Tuber is Gastrodine.Gastrodine extracts from the stem tuber of rhizoma Gastrodiae, and the injection liquid made with Gastrodine has calmness and the soporific function of highly significant, all has mitigation to symptoms such as neurasthenia, insomnia, headaches.But except Gastrodine, also have other critical function composition in Gastrodia Elata Stem Tuber as sky sesame oil, gastrodia elata polysaccharide and Rhizoma Gastrodiae starch etc.Traditional Gastrodine extractive technique is only focused on extracting Gastrodine, then often directly discarded for other functional components, causes the serious wasting of resources thus.Therefore, study rhizoma Gastrodiae medicinal ingredients and functional component comprehensive utilization extractive technique Rhizoma Gastrodiae scientific development is utilized, economize on resources, cut the waste significant.
Summary of the invention
For above-mentioned prior art Problems existing, the invention provides a kind of method simultaneously extracting sky sesame oil and Gastrodine from rhizoma Gastrodiae, the method technical process is simple, and easy to operate, cost is low, can extract day sesame oil and Gastrodine simultaneously.
Realizing the technical scheme that above-mentioned purpose of the present invention adopts is:
From rhizoma Gastrodiae, extract a method for sky sesame oil and Gastrodine simultaneously, comprise the steps:
1) first Gastrodia Elata Stem Tuber is pulverized, obtain Tall Gastrodis Tuber, Tall Gastrodis Tuber is joined in pressure pan, then in pressure pan, dehydrated alcohol is injected, after being uniformly mixed, be pressurized to 0.5-10MPa, be heated to 50-80 DEG C simultaneously, maintain constant temperature and pressure and extract after 2-10 hour, discharge the extraction feed liquid of gained after extracting in pressure pan, rejoin fresh dehydrated alcohol more again to extract, after recirculation extracts 3-5 time, collect each gained that extracts and extract feed liquid, obtain and always extract feed liquid, filter and always extract feed liquid, remove filter residue A, obtain filtrate A;
2) filtrate A is carried out vacuum decompression and reclaim ethanol, obtain a day sesame oil crude product;
3) sesame oil crude product water miscible extraction agent in sky is carried out stirring extraction, extraction temperature is 30-60 DEG C, and after stirring, leave standstill and be cooled to room temperature, until there is demixing phenomenon, upper strata is sky sesame oil, and lower floor is Gastrodine crude product A; Or at room temperature leave standstill sky sesame oil crude product until precipitation is complete, namely the oil reservoir collecting upper strata obtains day sesame oil, collects the precipitation of lower floor, obtains Gastrodine crude product B;
4) Gastrodine crude product A is carried out vacuum concentration, then extract with sherwood oil, after stratification, lower floor's aqueous phase is carried out vacuum concentration, drying, obtains pale powder; Or Gastrodine crude product B sherwood oil is extracted, after stratification, lower sediment is carried out vacuum-drying, obtains pale powder;
5) by step 4) the pale powder sherwood oil that obtains soaks 5-10 hour under the condition stirred, and soaking temperature is 50-70 DEG C, refilters, and removes liquor B and obtains filter residue B, dried by filter residue B, obtain Gastrodine.
Technique scheme is improved, step 2) in, the temperature that vacuum reclaims is 50-60 DEG C; Step 3) in, described extraction agent is pure water or volumn concentration is the ethanolic soln of 10%-50%; Step 4) in, after Gastrodine crude product A vacuum concentration to 1/10-1/5 volume, then extract with the sherwood oil of 5-10 times of volume; Step 4) in, the sherwood oil of Gastrodine crude product B 5-10 times of volume is extracted.
Compared with prior art, its beneficial effect and advantage are in the present invention:
1, the method organic solvent dehydrated alcohol extracts Tall Gastrodis Tuber, avoids the problem in the past causing the too much and sad filter of impurity with water extraction.
2, the method pure water or aqueous ethanolic solution carry out stirring to the sky sesame oil crude product obtained and extract, or are directly left standstill by sky sesame oil crude product, avoid the use of noxious solvent and poisonously to remain, thus avoiding the generation of waste water, very environmental protection and economy.
3, the method can isolate Gastrodine and sky sesame oil simultaneously, not only increases the efficiency of production, reduces production cost, and has saved resource, improves the utilization ratio of Rhizoma Gastrodiae, decreases waste.The more important thing is, test shows, the method increases the purity of Gastrodine.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet simultaneously extracting the method for sky sesame oil and Gastrodine from rhizoma Gastrodiae provided by the invention.
Fig. 2 is the schematic flow sheet of the method for traditional extraction Gastrodine.
Embodiment
Below in conjunction with specific embodiment, the present invention is specifically described.
Embodiment 1
1) first Gastrodia Elata Stem Tuber is pulverized, cross 100 object sieves, obtain Tall Gastrodis Tuber, the Tall Gastrodis Tuber of 500kg is joined 10m
3pressure pan in, then in pressure pan, inject the food-grade anhydrous ethanol of 5 times of volumes, open whipping appts, rotating speed is 500 revs/min, after being uniformly mixed, be pressurized to 0.5MPa, be heated to 60 DEG C simultaneously, after maintenance constant temperature and pressure extracts 2 hours, discharge the extraction feed liquid of gained after extracting in high pressure pipe, rejoin fresh dehydrated alcohol more again to extract, after recirculation extracts 3 times, collect each gained that extracts and extract feed liquid, obtain and always extract feed liquid, filter and always extract feed liquid, remove filter residue, obtain filtrate A.
2) filtrate A is carried out vacuum decompression recovery under the condition of 60 DEG C, after reclaiming ethanol, obtain a day sesame oil crude product.
3) sky sesame oil crude product pure water is carried out stirring extraction, the ratio of it sesame oil crude product and pure water is 2:1, extraction temperature is 60 DEG C, stirring velocity is 500 revs/min, and churning time is 1 hour, after stirring, leave standstill and be cooled to room temperature, until there is demixing phenomenon, upper strata is sky sesame oil, and lower floor is Gastrodine crude product.
4) after Gastrodine crude product being concentrated in vacuo to 1/10 volume, then extract with the sherwood oil of 8 times of volumes, after stratification, lower floor's aqueous phase is carried out vacuum concentration, drying, obtains pale powder.
5) soaked 5 hours under the condition stirred by pale powder sherwood oil, soaking temperature is 60 DEG C, refilters, and removes liquor B and obtains filter cake, dried by filter cake, obtain Gastrodine.
The method (concrete technology flow process as shown in Figure 2) that method of the present invention (concrete technology flow process as shown in Figure 1) and traditional Gastrodine extract is contrasted, method of the present invention is for embodiment 1, and two kinds of methods are to extract 1kg Gastrodine.
Concrete outcome is in table 1:
The method that table 1 method of the present invention and traditional Gastrodine extract extracts the contrast table of Gastrodine
As seen from the above table, compared with the extracting method of traditional Gastrodine, method of the present invention is adopted to extract Gastrodine, the required water yield is relatively less, and the amount of required ethanol is relatively many, but ethanol can all recyclings, the amount of required sherwood oil is suitable, required people's number is at most the half of traditional method, and coal consumption is 1/4 of traditional method, and the purity of gained Gastrodine is relatively high.In a word, it is low that the method extracts Gastrodine energy consumption, and cost of labor is low, and the purity of the Gastrodine of gained reaches 80%, and can also obtain day sesame oil.
Embodiment 2
1) first Gastrodia Elata Stem Tuber is pulverized, cross 100 object sieves, obtain Tall Gastrodis Tuber, the Tall Gastrodis Tuber of 500kg is joined 5m
3pressure pan in, then in pressure pan, inject the food-grade anhydrous ethanol of 5 times of volumes, open whipping appts, rotating speed is 500 revs/min, after being uniformly mixed, be pressurized to 5MPa, be heated to 50 DEG C simultaneously, after maintenance constant temperature and pressure extracts 6 hours, discharge the extraction feed liquid of gained after extracting in high pressure pipe, rejoin fresh dehydrated alcohol more again to extract, after recirculation extracts 4 times, collect each gained that extracts and extract feed liquid, obtain and always extract feed liquid, filter and always extract feed liquid, remove filter residue, obtain filtrate A.
2) filtrate A is carried out vacuum decompression recovery under the condition of 55 DEG C, after reclaiming ethanol, obtain a day sesame oil crude product.
3) sky sesame oil crude product is stirred extraction with carrying out 30% ethanolic soln, the ratio of it sesame oil crude product and ethanolic soln is 1:1, extraction temperature is 30 DEG C, stirring velocity is 500 revs/min, and churning time is 2 hours, after stirring, leave standstill and be cooled to room temperature, until there is demixing phenomenon, upper strata is sky sesame oil, and lower floor is Gastrodine crude product.
4) after Gastrodine crude product being concentrated in vacuo to 1/8 volume, then extract with the sherwood oil of 5 times of volumes, after stratification, lower floor's aqueous phase is carried out vacuum concentration, drying, obtains pale powder.
5) soaked 7 hours under the condition stirred by pale powder sherwood oil, soaking temperature is 70 DEG C, refilters, and removes liquor B and obtains filter cake, dried by filter cake, obtain Gastrodine.
Embodiment 3
1) first Gastrodia Elata Stem Tuber is pulverized, cross 100 object sieves, obtain Tall Gastrodis Tuber, the Tall Gastrodis Tuber of 500kg is joined in the pressure pan of 5m3, then in pressure pan, inject the food-grade anhydrous ethanol of 5 times of volumes, open whipping appts, rotating speed is 500 revs/min, after being uniformly mixed, be pressurized to 10MPa, be heated to 80 DEG C simultaneously, after maintenance constant temperature and pressure extracts 10 hours, discharge the extraction feed liquid of gained after extracting in high pressure pipe, rejoin fresh dehydrated alcohol more again to extract, after recirculation extracts 5 times, collect each gained that extracts and extract feed liquid, obtain and always extract feed liquid, filter and always extract feed liquid, remove filter residue, obtain filtrate A.
2) filtrate A is carried out vacuum decompression recovery under the condition of 50 DEG C, after reclaiming ethanol, obtain a day sesame oil crude product.
3) sky sesame oil crude product is stirred extraction with carrying out 50% ethanolic soln, the ratio of it sesame oil crude product and ethanolic soln is 1:1, extraction temperature is 50 DEG C, stirring velocity is 500 revs/min, and churning time is 1 hour, after stirring, leave standstill and be cooled to room temperature, until there is demixing phenomenon, upper strata is sky sesame oil, and lower floor is Gastrodine crude product.
4) after Gastrodine crude product being concentrated in vacuo to 1/5 volume, then extract with the sherwood oil of 10 times of volumes, after stratification, lower floor's aqueous phase is carried out vacuum concentration, drying, obtains pale powder.
5) soaked 10 hours under the condition stirred by pale powder sherwood oil, soaking temperature is 50 DEG C, refilters, and removes liquor B and obtains filter residue, dried by filter residue, obtain Gastrodine.
Embodiment 4
1) first Gastrodia Elata Stem Tuber is pulverized, cross 100 object sieves, obtain Tall Gastrodis Tuber, the Tall Gastrodis Tuber of 200kg is joined in the pressure pan of 2m3, then in pressure pan, inject the food-grade anhydrous ethanol of 10 times of volumes, open whipping appts, rotating speed is 500 revs/min, after being uniformly mixed, be pressurized to 6MPa, be heated to 60 DEG C simultaneously, after maintenance constant temperature and pressure extracts 3 hours, discharge the extraction feed liquid of gained after extracting in high pressure pipe, rejoin fresh dehydrated alcohol more again to extract, after recirculation extracts 3 times, collect each gained that extracts and extract feed liquid, obtain and always extract feed liquid, filter and always extract feed liquid, remove filter residue, obtain filtrate A.
2) filtrate A is carried out vacuum decompression recovery under the condition of 60 DEG C, after reclaiming ethanol, obtain a day sesame oil crude product.
3) or by sky sesame oil crude product at room temperature leave standstill until precipitation is complete, collecting precipitation after removal supernatant liquid, obtains Gastrodine crude product.
4) or by the sherwood oil of Gastrodine crude product with 6 times extract, after stratification, lower floor's aqueous phase is carried out vacuum concentration, drying, obtains pale powder.
5) soaked 10 hours under the condition stirred by pale powder sherwood oil, soaking temperature is 50 DEG C, refilters, and removes liquor B and obtains filter cake, dried by filter cake, obtain Gastrodine.
The method (concrete technology flow process as shown in Figure 2) method of the present invention and traditional Gastrodine extracted contrasts, and method of the present invention is for embodiment 4, and two kinds of methods are to extract 1kg Gastrodine.
Concrete outcome is in table 2:
The method that table 2 method of the present invention and traditional Gastrodine extract extracts the contrast table of Gastrodine
As seen from the above table, compared with the extracting method of traditional Gastrodine, method of the present invention is adopted to extract Gastrodine, the required water yield is relatively less, and the amount of required ethanol is relatively many, but ethanol can all recyclings, the amount of required sherwood oil is suitable, required people's number is at most 1/3rd of traditional method, and coal consumption is 1/4 of traditional method, and the purity of gained Gastrodine significantly improves.In a word, it is low that the method extracts Gastrodine energy consumption, and cost of labor is low, and the purity of the Gastrodine of gained more than 80%, and can also obtain day sesame oil.
Claims (5)
1. from rhizoma Gastrodiae, extract a method for sky sesame oil and Gastrodine simultaneously, it is characterized in that comprising the steps:
1) first Gastrodia Elata Stem Tuber is pulverized, obtain Tall Gastrodis Tuber, Tall Gastrodis Tuber is joined in pressure pan, then in pressure pan, dehydrated alcohol is injected, after being uniformly mixed, be pressurized to 0.5-10MPa, be heated to 50-80 DEG C simultaneously, maintain constant temperature and pressure and extract after 2-10 hour, discharge the extraction feed liquid of gained after extracting in pressure pan, rejoin fresh dehydrated alcohol more again to extract, after recirculation extracts 3-5 time, collect each gained that extracts and extract feed liquid, obtain and always extract feed liquid, filter and always extract feed liquid, remove filter residue A, obtain filtrate A;
2) filtrate A is carried out vacuum decompression and reclaim ethanol, obtain a day sesame oil crude product;
3) sesame oil crude product water miscible extraction agent in sky is carried out stirring extraction, extraction temperature is 30-60 DEG C, and after stirring, leave standstill and be cooled to room temperature, until there is demixing phenomenon, upper strata is sky sesame oil, and lower floor is Gastrodine crude product A; Or at room temperature leave standstill sky sesame oil crude product until precipitation is complete, namely the oil reservoir collecting upper strata obtains day sesame oil, collects the precipitation of lower floor, obtains Gastrodine crude product B;
4) Gastrodine crude product A is carried out vacuum concentration, then extract with sherwood oil, after stratification, lower floor's aqueous phase is carried out vacuum concentration, drying, obtains pale powder; Or Gastrodine crude product B sherwood oil is extracted, after stratification, lower sediment is carried out vacuum-drying, obtains pale powder;
5) by step 4) the pale powder sherwood oil that obtains soaks 5-10 hour under the condition stirred, and soaking temperature is 50-70 DEG C, refilters, and removes liquor B and obtains filter residue B, dried by filter residue B, obtain Gastrodine.
2. the method simultaneously extracting sky sesame oil and Gastrodine from rhizoma Gastrodiae according to claim 1, is characterized in that: step 2) in, the temperature that vacuum reclaims is 50-60 DEG C.
3. the method simultaneously extracting sky sesame oil and Gastrodine from rhizoma Gastrodiae according to claim 1, is characterized in that: step 3) in, described extraction agent is pure water or volumn concentration is the ethanolic soln of 10%-50%.
4. the method simultaneously extracting sky sesame oil and Gastrodine from rhizoma Gastrodiae according to claim 1, is characterized in that: step 4) in, after Gastrodine crude product A vacuum concentration to 1/10-1/5 volume, then extract with the sherwood oil of 5-10 times of volume.
5. the method simultaneously extracting sky sesame oil and Gastrodine from rhizoma Gastrodiae according to claim 1, is characterized in that: step 4) in, the sherwood oil of Gastrodine crude product B 5-10 times of volume is extracted.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106986904A (en) * | 2017-05-08 | 2017-07-28 | 铜仁学院 | A kind of Gastrodin extracted in the anesthesia stem from day and preparation method thereof |
| CN108409808A (en) * | 2018-05-31 | 2018-08-17 | 中山大学 | A kind of method of the broken extraction Gastrodin in Gastrodia eleta Bl. of continuous low-temperature high pressure |
| CN111035009A (en) * | 2018-10-15 | 2020-04-21 | 南漳致远农业科技有限公司 | Method for producing gastrodia elata paste by using gastrodia elata waste materials |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102988783A (en) * | 2012-12-30 | 2013-03-27 | 贵州大方百里花食品有限公司 | Production method of gastrodin |
| CN103242461A (en) * | 2012-02-06 | 2013-08-14 | 陕西理工学院 | Novel method for simultaneously extracting gastrodia elata polysaccharide and gastrodine |
| CN103896999A (en) * | 2014-04-15 | 2014-07-02 | 贵州大学 | Preparation method of parishin reference substance |
-
2015
- 2015-11-26 CN CN201510833959.8A patent/CN105348334B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242461A (en) * | 2012-02-06 | 2013-08-14 | 陕西理工学院 | Novel method for simultaneously extracting gastrodia elata polysaccharide and gastrodine |
| CN102988783A (en) * | 2012-12-30 | 2013-03-27 | 贵州大方百里花食品有限公司 | Production method of gastrodin |
| CN103896999A (en) * | 2014-04-15 | 2014-07-02 | 贵州大学 | Preparation method of parishin reference substance |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106986904A (en) * | 2017-05-08 | 2017-07-28 | 铜仁学院 | A kind of Gastrodin extracted in the anesthesia stem from day and preparation method thereof |
| CN108409808A (en) * | 2018-05-31 | 2018-08-17 | 中山大学 | A kind of method of the broken extraction Gastrodin in Gastrodia eleta Bl. of continuous low-temperature high pressure |
| CN108409808B (en) * | 2018-05-31 | 2021-04-06 | 中山大学 | Method for continuously extracting gastrodin from gastrodia elata through low-temperature high-pressure crushing |
| CN111035009A (en) * | 2018-10-15 | 2020-04-21 | 南漳致远农业科技有限公司 | Method for producing gastrodia elata paste by using gastrodia elata waste materials |
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