CN115068520A - Bitter removing method for primary cistanche pulp - Google Patents
Bitter removing method for primary cistanche pulp Download PDFInfo
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- CN115068520A CN115068520A CN202210649041.8A CN202210649041A CN115068520A CN 115068520 A CN115068520 A CN 115068520A CN 202210649041 A CN202210649041 A CN 202210649041A CN 115068520 A CN115068520 A CN 115068520A
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- 241000005787 Cistanche Species 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000012528 membrane Substances 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 24
- 238000001728 nano-filtration Methods 0.000 claims abstract description 22
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 17
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 17
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 17
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 17
- 229960004853 betadex Drugs 0.000 claims abstract description 17
- 229940093429 polyethylene glycol 6000 Drugs 0.000 claims abstract description 17
- 238000001556 precipitation Methods 0.000 claims abstract description 15
- 239000006228 supernatant Substances 0.000 claims abstract description 15
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 102000004190 Enzymes Human genes 0.000 claims abstract description 11
- 108090000790 Enzymes Proteins 0.000 claims abstract description 11
- 230000009849 deactivation Effects 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims description 14
- 239000012530 fluid Substances 0.000 claims description 14
- 239000012466 permeate Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 8
- 239000013049 sediment Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 2
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims 2
- 239000000126 substance Substances 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 3
- 241000336291 Cistanche deserticola Species 0.000 abstract description 2
- 229940126680 traditional chinese medicines Drugs 0.000 abstract description 2
- 210000000805 cytoplasm Anatomy 0.000 description 7
- 150000004676 glycans Chemical class 0.000 description 6
- 229930182470 glycoside Natural products 0.000 description 6
- 150000002338 glycosides Chemical class 0.000 description 6
- 229920001282 polysaccharide Polymers 0.000 description 6
- 239000005017 polysaccharide Substances 0.000 description 6
- 230000001954 sterilising effect Effects 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 235000013361 beverage Nutrition 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 241000308150 Orobanchaceae Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003071 parasitic effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/64—Orobanchaceae (Broom-rape family)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
- A61K47/10—Alcohols; Phenols; Salts thereof, e.g. glycerol; Polyethylene glycols [PEG]; Poloxamers; PEG/POE alkyl ethers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
- A61K47/40—Cyclodextrins; Derivatives thereof
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Public Health (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Veterinary Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Inorganic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to the technical field of deep processing of traditional Chinese medicines, in particular to a method for removing bitter of primary cistanche pulp, which comprises the following steps: filtering and removing impurities from the primary pulp of cistanche deserticola, concentrating, carrying out ultrahigh temperature instant enzyme deactivation, adding ethanol into the concentrated primary pulp, carrying out alcohol precipitation, separating supernatant from bottom layer liquid containing precipitate, passing the supernatant through a nanofiltration membrane to obtain ethanol filtrate and trapped liquid, repeating the steps for 4-6 times, adding beta-cyclodextrin and polyethylene glycol 6000, embedding bitter components into molecules of the ethanol filtrate and the trapped liquid by utilizing the beta-cyclodextrin and the polyethylene glycol 6000, mixing and stirring, and carrying out ultrafiltration through an ultrafiltration membrane to recover the permeated liquid; in the whole process of the invention, the content of bitter substances is reduced, thereby realizing the bitter-removing effect.
Description
Technical Field
The invention relates to the technical field of deep processing of traditional Chinese medicines, in particular to a method for removing bitter of cistanche primary pulp.
Background
Cistanche deserticola is a perennial whole parasitic herb plant of cistanche genus of the family Orobanchaceae, has the efficacies of tonifying kidney and strengthening yang, replenishing essence and benefiting marrow, relaxing bowel and the like, and is recorded in the calendar pharmacopoeia. A large number of researches show that the cistanche has various effects in the aspect of medical care and has large market demand.
In the deep processing of the cistanche, the traditional Chinese medicine beverage taking the cistanche as the raw material is popular in the market due to the advantages of convenient drinking and easy absorption, but the cistanche is slightly bitter and has poor taste, and the quality of the cistanche beverage is greatly reduced.
Disclosure of Invention
In view of the above, the present invention aims to overcome the defects in the prior art, and provides a method for debitterizing primary cistanche pulp, which comprises the following steps:
(1) filtering a batch of cistanche original pulp to remove impurities, concentrating, and performing ultrahigh-temperature instant enzyme deactivation at the temperature of 135-141 ℃.
(2) Standing and cooling the concentrated original pulp of cistanche after enzyme deactivation, adding ethanol with volume fraction of 95% which is 5-10 times of the volume of the cooled concentrated original pulp, carrying out alcohol precipitation, separating supernatant and bottom layer liquid containing precipitate, and separating polysaccharide in the concentrated original pulp.
(3) And (3) passing the supernatant through a nanofiltration membrane to obtain an ethanol filtrate and trapped fluid, wherein the polysaccharide with larger molecular weight is separated in advance, so that the filtration membrane is not easy to block during nanofiltration, and the ethanol filtrate can be reused for alcohol precipitation after purification, thereby reducing consumption.
(4) And (3) concentrating bitter substances in the trapped liquid because the bitter substances cannot pass through the nano-filtration membrane with the micro-aperture, merging the bitter substances into the primary cistanche pulp of the next batch, and repeating the steps (1) to (3).
(5) Repeating the steps (1) - (4) for 4-6 times, increasing the enrichment degree of bitter substances, diluting with pure water, adding beta-cyclodextrin and polyethylene glycol 6000 into the diluent, embedding bitter components into molecules by utilizing the beta-cyclodextrin and the polyethylene glycol 6000, mixing and stirring, performing ultrafiltration by using an ultrafiltration membrane, recovering a permeate, wherein the permeate contains a large amount of phenylethanoid glycosides, and the permeate and a precipitate-containing bottom layer liquid are used as subsequent processing raw materials.
The molecular weight cut-off of the nanofiltration membrane is between 150 and 250Da, the nanofiltration membrane is operated under the condition of pressurization or normal pressure, and the operation temperature is maintained at normal temperature or below.
The mass percentage of the beta-cyclodextrin and the polyethylene glycol 6000 in the step (4) is (5-20): 1.
the mass percentage of the beta-cyclodextrin and the polyethylene glycol 6000 is 10: 1.
the cutoff molecular weight of the ultrafiltration membrane is between 1000 and 2000Da, the ultrafiltration membrane is operated under the condition of pressurization or normal pressure, and pure water is used for washing and filtering.
The invention has the beneficial effects that: the invention discloses a method for debitterizing cistanche protoplasm, which comprises the steps of firstly precipitating macromolecular polysaccharide by using alcohol precipitation, performing nanofiltration to recover an ethanol raw material, enriching bitter substances, embedding odor substances in final trapped liquid by using beta-cyclodextrin and polyethylene glycol 6000 after repeated times, performing ultrafiltration by using an ultrafiltration membrane to obtain a permeate containing phenylethanoid glycosides, and taking the permeate and the alcohol precipitated substances as raw materials for subsequent processing; in the whole process, the content of bitter substances is reduced, thereby realizing the bitter-removing effect.
Drawings
The invention is further described below with reference to the following figures and examples:
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
As shown in fig. 1
Filtering 100kg of cistanche original pulp to remove impurities, concentrating to half of the original volume, feeding into an industrial ultrahigh-temperature instant sterilization device, and performing ultrahigh-temperature instant enzyme deactivation at 135-141 ℃.
Standing and cooling the concentrated cistanche protoplasm after enzyme deactivation, or cooling and accelerating the cooling speed, adding ethanol with the volume fraction of 95% which is 5 times of the volume of the concentrated cistanche protoplasm after cooling, carrying out alcohol precipitation, standing overnight, separating supernatant liquid from bottom layer liquid containing precipitate, and carrying out a further debittering step on the supernatant liquid, wherein the bottom layer liquid containing precipitate does not need further debittering due to the high polysaccharide content.
And (2) enabling the supernatant to pass through a nanofiltration membrane, wherein the molecular weight cut-off of the nanofiltration membrane is between 150 and 250Da, the nanofiltration membrane is operated under pressurization, the operation temperature is kept at a normal temperature and is set at a lower level, an ethanol filtrate and a cut-off solution are obtained, and the ethanol filtrate is purified and then is reused for alcohol precipitation.
And (4) merging the trapped fluid into the next batch of cistanche original pulp, repeating alcohol precipitation and nanofiltration processes, continuously enriching bitter substances and phenylethanoid glycosides in the trapped fluid, and further processing the final trapped fluid after repeating enrichment for 6 times.
Specifically, the trapped fluid is diluted by pure water, beta-cyclodextrin and polyethylene glycol 6000 are added into the diluted fluid, and the mass percentage of the beta-cyclodextrin to the polyethylene glycol 6000 is 5: 1, using a special molecular hole structure of beta-cyclodextrin and the solubilizing effect of polyethylene glycol 6000 to include bitter and astringent components, mixing and stirring, then performing ultrafiltration by an ultrafiltration membrane, wherein the cut-off molecular weight of the ultrafiltration membrane is between 1000 and 2000Da, the included bitter and astringent components cannot pass through, the phenylethanoid glycosides can be filtered, recovering a permeate, using the permeate and a sediment-containing bottom layer liquid as subsequent processing raw materials, performing ultrafiltration under the condition of pressurization or normal pressure, and performing washing and filtration by using pure water.
Example two
Filtering 100kg of cistanche original pulp to remove impurities, concentrating to half of the original volume, feeding into an industrial ultrahigh-temperature instant sterilization device, and performing ultrahigh-temperature instant enzyme deactivation at 135-141 ℃.
Standing and cooling the concentrated cistanche protoplasm after enzyme deactivation, or cooling and accelerating the cooling speed, adding ethanol with the volume fraction of 95% which is 10 times of the volume of the concentrated cistanche protoplasm after cooling, carrying out alcohol precipitation, standing overnight, separating supernatant liquid from sediment-containing bottom layer liquid, and carrying out a further debittering step on the supernatant liquid, wherein the sediment-containing bottom layer liquid does not need further debittering due to high polysaccharide content.
And (2) enabling the supernatant to pass through a nanofiltration membrane, wherein the molecular weight cut-off of the nanofiltration membrane is between 150 and 250Da, the nanofiltration membrane is operated under normal pressure, the operation temperature is maintained at a normal temperature and is set at a lower level, an ethanol filtrate and a cut-off solution are obtained, and the ethanol filtrate is purified and then is reused for alcohol precipitation.
And (4) merging the trapped liquid into the next batch of cistanche primary pulp, repeating alcohol precipitation and nanofiltration processes, continuously enriching bitter substances and phenylethanoid glycosides in the trapped liquid, and further processing the final trapped liquid after repeating enrichment for 4 times.
Specifically, the trapped fluid is diluted by pure water, beta-cyclodextrin and polyethylene glycol 6000 are added into the diluted fluid, and the mass percentage of the beta-cyclodextrin to the polyethylene glycol 6000 is 10: 1, mixing, stirring, performing ultrafiltration by an ultrafiltration membrane, wherein the cutoff molecular weight of the ultrafiltration membrane is between 1000 and 2000Da, recovering a permeate, using the permeate and a sediment-containing bottom layer liquid as subsequent processing raw materials, performing ultrafiltration under a pressurized or normal pressure condition, and performing washing filtration by using pure water.
EXAMPLE III
Filtering 100kg of cistanche original pulp to remove impurities, concentrating to half of the original volume, feeding into an industrial ultrahigh-temperature instant sterilization device, and performing ultrahigh-temperature instant enzyme deactivation at 135-141 ℃.
Standing and cooling the concentrated cistanche protoplasm after enzyme deactivation, or cooling and accelerating the cooling speed, adding ethanol with the volume fraction of 95% which is 10 times of the volume of the concentrated cistanche protoplasm after cooling, carrying out alcohol precipitation, standing overnight, separating supernatant liquid from sediment-containing bottom layer liquid, and carrying out a further debittering step on the supernatant liquid, wherein the sediment-containing bottom layer liquid does not need further debittering due to high polysaccharide content.
And (2) enabling the supernatant to pass through a nanofiltration membrane, wherein the molecular weight cut-off of the nanofiltration membrane is between 150 and 250Da, the nanofiltration membrane is operated under normal pressure, the operation temperature is maintained at a normal temperature and is set at a lower level, an ethanol filtrate and a cut-off solution are obtained, and the ethanol filtrate is purified and then is reused for alcohol precipitation.
And (4) merging the trapped liquid into the next batch of cistanche primary pulp, repeating alcohol precipitation and nanofiltration processes, continuously enriching bitter substances and phenylethanoid glycosides in the trapped liquid, and further processing the final trapped liquid after repeating enrichment for 4 times.
Specifically, the trapped fluid is diluted by pure water, beta-cyclodextrin and polyethylene glycol 6000 are added into the diluted fluid, and the mass percentage of the beta-cyclodextrin to the polyethylene glycol 6000 is 20: 1, mixing, stirring, performing ultrafiltration by an ultrafiltration membrane, wherein the cutoff molecular weight of the ultrafiltration membrane is between 1000 and 2000Da, recovering a permeate, using the permeate and a sediment-containing bottom layer liquid as subsequent processing raw materials, performing ultrafiltration under a pressurized or normal pressure condition, and performing washing filtration by using pure water.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (5)
1. A method for debitterizing primary cistanche pulp is characterized by comprising the following steps: the method comprises the following steps:
(1) filtering a batch of primary cistanche juice to remove impurities, concentrating, and performing ultrahigh-temperature instant enzyme deactivation at the temperature of 135-141 ℃;
(2) standing and cooling the concentrated original pulp of cistanche after enzyme deactivation, adding ethanol with volume fraction of 95% which is 5-10 times of the volume of the cooled concentrated original pulp, carrying out alcohol precipitation, and separating supernatant and bottom layer liquid containing precipitate;
(3) passing the supernatant through a nanofiltration membrane to obtain an ethanol filtrate and trapped fluid, and purifying the ethanol filtrate for alcohol precipitation;
(4) the trapped fluid is merged into the primary cistanche juice of the next batch, and the steps (1) to (3) are repeated;
(5) and (3) repeating the steps (1) to (4) for 4-6 times, diluting the trapped fluid with pure water, adding beta-cyclodextrin and polyethylene glycol 6000 into the diluted fluid, mixing and stirring, performing ultrafiltration through an ultrafiltration membrane, recovering the permeate, and taking the permeate and the sediment-containing bottom layer solution as subsequent processing raw materials.
2. The method for debitterizing primary cistanche pulp according to claim 1, which is characterized by comprising the following steps: the molecular weight cut-off of the nanofiltration membrane is between 150 and 250Da, the nanofiltration membrane is operated under the condition of pressurization or normal pressure, and the operation temperature is maintained at normal temperature or below.
3. The method for debitterizing primary cistanche pulp according to claim 1, which is characterized by comprising the following steps: the mass percentage of the beta-cyclodextrin and the polyethylene glycol 6000 in the step (4) is (5-20): 1.
4. the method for debitterizing primary cistanche pulp according to claim 3, which is characterized by comprising the following steps: the mass percentage of the beta-cyclodextrin and the polyethylene glycol 6000 is 10: 1.
5. the method for debitterizing primary cistanche pulp according to claim 1, which is characterized by comprising the following steps: the cutoff molecular weight of the ultrafiltration membrane is between 1000 and 2000Da, the ultrafiltration membrane is operated under the condition of pressurization or normal pressure, and pure water is used for washing and filtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210649041.8A CN115068520A (en) | 2022-06-09 | 2022-06-09 | Bitter removing method for primary cistanche pulp |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210649041.8A CN115068520A (en) | 2022-06-09 | 2022-06-09 | Bitter removing method for primary cistanche pulp |
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| Publication Number | Publication Date |
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| CN115068520A true CN115068520A (en) | 2022-09-20 |
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| CN202210649041.8A Pending CN115068520A (en) | 2022-06-09 | 2022-06-09 | Bitter removing method for primary cistanche pulp |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041677A (en) * | 2007-04-23 | 2007-09-26 | 和田帝辰医药生物科技有限公司 | Producing raw material containing benzyl carbinol glycosides from Cistanche deserticola by using membrane separation technique and preparation method thereof |
| CN101214282A (en) * | 2007-12-28 | 2008-07-09 | 中山大学 | Method for extracting active component from cistanche salsa |
| CN114515008A (en) * | 2022-03-04 | 2022-05-20 | 广东青云山药业有限公司 | Cistanche tubulosa extract and preparation method thereof |
-
2022
- 2022-06-09 CN CN202210649041.8A patent/CN115068520A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041677A (en) * | 2007-04-23 | 2007-09-26 | 和田帝辰医药生物科技有限公司 | Producing raw material containing benzyl carbinol glycosides from Cistanche deserticola by using membrane separation technique and preparation method thereof |
| CN101214282A (en) * | 2007-12-28 | 2008-07-09 | 中山大学 | Method for extracting active component from cistanche salsa |
| CN114515008A (en) * | 2022-03-04 | 2022-05-20 | 广东青云山药业有限公司 | Cistanche tubulosa extract and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王优杰等: "药物掩味技术的研发进展与应用", 中国药学杂志 * |
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Application publication date: 20220920 |