CN103981018B - A kind of preparation method of Ganoderma spore oil - Google Patents
A kind of preparation method of Ganoderma spore oil Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of Ganoderma spore oil, it is characterized in that adopting following steps: A: first Ganoderma spore powder is dried, pulverize, carry out broken wall treatment by high pressure homogenizer, lyophilize, obtain Ganoderma spore powder; B: the dextrin of Ganoderma spore powder and 5%-8% is mixed and made into 20-50 object particle; C: by the particle prepared by step B, loads CO
2in supercritical extraction reactor, extract as entrainment agent with squalane, extract is purified through the first separating still and the second separating still successively, separating pressure 8-10MPa in first separating still, temperature 30-40 DEG C, the separating pressure in the second separating still is 5-8MPa, and temperature is 20 ~ 30 DEG C, from the second separating still extract out, be Ganoderma spore oil.The present invention has Ganoderma powder sporoderm-broken rate and is greater than 98%, and ganoderma spore oil yield is higher than 35%, and total triterpene contents is at the beneficial effect of 3-5%.
Description
Technical field
The present invention relates to the separation and extraction technology of natural product effective ingredient, particularly a kind of preparation method of Ganoderma spore oil.
Background technology
Ganoderma spore is the sexual reproductive cell of glossy ganoderma, whole genetic activities materials containing glossy ganoderma, have antitumor, the effect such as blood sugar and immunomodulatory, in pharmacology with there is application clinically, also be a kind of good natural health-care products starting material, be mainly used in anti-aging product at cosmetic field.Ganoderma lucidum triterpene compounds is present in Ganoderma spore oil, it is the main functional component of Ganoderma spore, but Ganoderma spore wall has two-layer, inner containing 1-2 oil droplet, outer wall is made up of chitin mass shell, insoluble fibre and the xylogen that one deck is hard, there is very strong resistance to acids and bases, prevent solvent to the extraction of Ganoderma spore oil.The extracting method of current Ganoderma spore oil mainly contains the methods such as acid-base method, enzymolysis process, microwave method, supersonic method, liquid nitrogen quenching method, although can improve Ganoderma spore oil yield, working (machining) efficiency is low, and cost is high, be only applicable to laboratory operation, be difficult to realize suitability for industrialized production.Patent CN 102973616 A " a kind of high biological activity Ganoderma spore oil and supercritical preparation process thereof ", adopts the impact grinding of high energy nanometer by ganoderma lucidium spore powder wall breaking, then in conjunction with supercritical CO
2extraction and molecular distillation purifying.This method prepares Ganoderma spore oil, and Ganoderma powder sporoderm-broken rate is not higher than 95%, and oil yield is about 30%, and total triterpene contents is at 2-3%.The content of effective constituent and purity in Ganoderma spore oil, relative traditional method increases, but Ganoderma powder sporoderm-broken rate, oil yield and total triterpene contents are all not high enough.
Summary of the invention
The object of this invention is to provide a kind of preparation method of Ganoderma spore oil, have the following advantages: Ganoderma powder sporoderm-broken rate is greater than 98%, ganoderma spore oil yield is higher than 35%, and total triterpene contents is at 3-5%.
For solving the problems of the technologies described above, the present invention by the following technical solutions: a kind of preparation method of Ganoderma spore oil, it is characterized in that adopt following steps:
A: first Ganoderma spore powder is dried in 40-45 DEG C of baking oven, meal pulverized to obtain by pulverizer, the ratio of meal and dehydrated alcohol liquor ratio 1:5-10 is according to quantity mixed, broken wall treatment is carried out by high pressure homogenizer under normal temperature, 70 ~ 150Mpa pressure, then by the lyophilize in Freeze Drying Equipment of gained mixed solution, Ganoderma spore powder is obtained;
B: mixed with the dextrin of 5%-8% by Ganoderma spore powder, adopts nodulizer dry method under 5 Mpa to be pressed into 20-50 object particle;
C: by the particle prepared by step B, loads CO
2in supercritical extraction reactor, at CO
2the entrance and exit of supercritical extraction reactor arranges filter paper or absorbent cotton, stops particle when extracting to pass CO
2the screen plate of supercritical extraction reactor, extraction temperature is 40 ~ 50 DEG C, and extracting pressure is 30 ~ 45Mpa, and squalane is as entrainment agent, and the addition of squalane is 5 ~ 10%, CO of extraction kettle miospore opaque amount
2flow control at 200 ~ 400L/h, extraction time 2 ~ 3h; Extract is purified through the first separating still and the second separating still successively, the separating pressure 8-10MPa in the first separating still, temperature 30-40 DEG C, separating pressure in second separating still is 5-8MPa, temperature is 20 ~ 30 DEG C, from the second separating still extract out, is Ganoderma spore oil.
The present invention carries out broken wall by high pressure homogenizer, and using squalane as entrainment agent, by SCF-CO 2 Ganoderma spore oil, the Ganoderma spore oil of preparation is transparent homogeneous, can directly add in cosmetic formulations, Ganoderma powder sporoderm-broken rate is higher than 98%, and ganoderma spore oil yield is more than or equal to 35%, and total triterpene contents is at 3-5%.Compared with prior art, Ganoderma powder sporoderm-broken rate, ganoderma spore oil yield, total triterpene contents are all significantly improved.
In sum, preparation method of the present invention has Ganoderma powder sporoderm-broken rate and is greater than 98%, and ganoderma spore oil yield is higher than 35%, and total triterpene contents is at the beneficial effect of 3-5%.
Embodiment
The present invention is further illustrated by the following examples.
Embodiment 1:
A preparation method for Ganoderma spore oil, adopts following steps preparation:
A: first Ganoderma spore powder is dried in 45 DEG C of baking ovens, meal pulverized to obtain by pulverizer, the ratio of meal and dehydrated alcohol liquor ratio 1:5 is according to quantity mixed, broken wall treatment is carried out by high pressure homogenizer under normal temperature, 70Mpa pressure, then by the lyophilize in Freeze Drying Equipment of gained mixed solution, Ganoderma spore powder is obtained;
B: by Ganoderma spore powder with 5% dextrin mix, adopt nodulizer dry method under 5 Mpa to be pressed into 20 object particles;
C: by the particle prepared by step B, loads CO
2in supercritical extraction reactor, at CO
2the entrance and exit of supercritical extraction reactor arranges filter paper or absorbent cotton, stops particle when extracting to pass CO
2the screen plate of supercritical extraction reactor, extraction temperature is 40 DEG C, and extracting pressure is 30Mpa, and squalane is as entrainment agent, and the addition of squalane is the 5%(mass ratio of extraction kettle miospore opaque amount), CO
2flow control at 200L/h, extraction time 2h; Extract is purified through the first separating still and the second separating still successively, the separating pressure 8MPa in the first separating still, temperature 30 DEG C, and in the second separating still, separating pressure is 5MPa, and temperature is 20 DEG C, from the second separating still extract out, is Ganoderma spore oil.Prepared spore oil is transparent homogeneous, directly can add in cosmetic formulations and use.Ganoderma spore oil extraction yield is 35.4%, and detect Ganoderma powder sporoderm-broken rate is 98.3%, total triterpene contents is 3.5%.
Embodiment 2:
A preparation method for Ganoderma spore oil, adopts following steps preparation:
A: first Ganoderma spore powder is dried in 40 DEG C of baking ovens, meal pulverized to obtain by pulverizer, the ratio of meal and dehydrated alcohol liquor ratio 1:7 is according to quantity mixed, broken wall treatment is carried out by high pressure homogenizer under normal temperature, 80Mpa pressure, then by the lyophilize in Freeze Drying Equipment of gained mixed solution, Ganoderma spore powder is obtained;
B: by Ganoderma spore powder with 6% dextrin mix, adopt nodulizer dry method under 5 Mpa to be pressed into 30 object particles;
C: by the particle prepared by step B, loads CO
2in supercritical extraction reactor, at CO
2the entrance and exit of supercritical extraction reactor arranges filter paper or absorbent cotton, stops particle when extracting to pass CO
2the screen plate of supercritical extraction reactor, extraction temperature is 45 DEG C, and extracting pressure is 35Mpa, and squalane is as entrainment agent, and the addition of squalane is the 7%(mass ratio of extraction kettle miospore opaque amount), the flow control of CO2 at 300L/h, extraction time 2.5h; Extract is purified through the first separating still and the second separating still successively, the separating pressure 8MPa in the first separating still, temperature 30 DEG C, and in the second separating still, separating pressure is 6MPa, and temperature is 25 DEG C, from the second separating still extract out, is Ganoderma spore oil.Prepared spore oil is transparent homogeneous, directly can add in cosmetic formulations and use.Ganoderma spore oil extraction yield is 35.8%, and detect Ganoderma powder sporoderm-broken rate is 98.7%, total triterpene contents is 4.0%.
Embodiment 3:
A preparation method for Ganoderma spore oil, adopts following steps preparation:
A: first Ganoderma spore powder is dried in 45 DEG C of baking ovens, meal pulverized to obtain by pulverizer, the ratio of meal and dehydrated alcohol liquor ratio 1:10 is according to quantity mixed, broken wall treatment is carried out by high pressure homogenizer under normal temperature, 120Mpa pressure, then by the lyophilize in Freeze Drying Equipment of gained mixed solution, Ganoderma spore powder is obtained;
B: by Ganoderma spore powder with 8% dextrin mix, adopt nodulizer dry method under 5 Mpa to be pressed into 30 object particles;
C: by the particle prepared by step B, loads CO
2in supercritical extraction reactor, at CO
2the entrance and exit of supercritical extraction reactor arranges filter paper or absorbent cotton, stops particle when extracting to pass CO
2the screen plate of supercritical extraction reactor, extraction temperature is 45 DEG C, and extracting pressure is 40Mpa, and squalane is as entrainment agent, and the addition of squalane is the 10%(mass ratio of extraction kettle miospore opaque amount), the flow control of CO2 at 400L/h, extraction time 3h; Extract is purified through the first separating still and the second separating still successively, the separating pressure 10MPa in the first separating still, temperature 35 DEG C, and in the second separating still, separating pressure is 8MPa, and temperature is 20 DEG C, from the second separating still extract out, is Ganoderma spore oil.Prepared spore oil is transparent homogeneous, directly can add in cosmetic formulations and use.Ganoderma spore oil extraction yield is 36.5%, and detect Ganoderma powder sporoderm-broken rate is 98.8%, total triterpene contents is 5.0%.
Embodiment 4:
A preparation method for Ganoderma spore oil, adopts following steps preparation:
A: first Ganoderma spore powder is dried in 45 DEG C of baking ovens, meal pulverized to obtain by pulverizer, the ratio of meal and dehydrated alcohol liquor ratio 1:8 is according to quantity mixed, broken wall treatment is carried out by high pressure homogenizer under normal temperature, 150Mpa pressure, then by the lyophilize in Freeze Drying Equipment of gained mixed solution, Ganoderma spore powder is obtained;
B: by Ganoderma spore powder with 7% dextrin mix, adopt nodulizer dry method under 5 Mpa to be pressed into 40 object particles;
C: by the particle prepared by step B, loads CO
2in supercritical extraction reactor, at CO
2the entrance and exit of supercritical extraction reactor arranges filter paper or absorbent cotton, stops particle when extracting to pass CO
2the screen plate of supercritical extraction reactor, extraction temperature is 50 DEG C, and extracting pressure is 45Mpa, and squalane is as entrainment agent, and the addition of squalane is the 10%(mass ratio of extraction kettle miospore opaque amount), CO
2flow control at 400L/h, extraction time 2.5h; Extract is purified through the first separating still and the second separating still successively, the separating pressure 9MPa in the first separating still, temperature 40 DEG C, and in the second separating still, separating pressure is 7MPa, and temperature is 30 DEG C; From the second separating still extract out, be Ganoderma spore oil.Prepared spore oil is transparent homogeneous, directly can add in cosmetic formulations and use.Ganoderma spore oil extraction yield is 36.5%, and detect Ganoderma powder sporoderm-broken rate is 99.5%, total triterpene contents is 4.8%.
Embodiment 5:
A preparation method for Ganoderma spore oil, adopts following steps preparation:
A: first Ganoderma spore powder is dried in 45 DEG C of baking ovens, meal pulverized to obtain by pulverizer, the ratio of meal and dehydrated alcohol liquor ratio 1:8 is according to quantity mixed, broken wall treatment is carried out by high pressure homogenizer under normal temperature, 120Mpa pressure, then by the lyophilize in Freeze Drying Equipment of gained mixed solution, Ganoderma spore powder is obtained;
B: by Ganoderma spore powder with 8% dextrin mix, adopt nodulizer dry method under 5 Mpa to be pressed into 50 object particles;
C: by the particle prepared by step B, loads CO
2in supercritical extraction reactor, at CO
2the entrance and exit of supercritical extraction reactor arranges filter paper or absorbent cotton, stops particle when extracting to pass CO
2the screen plate of supercritical extraction reactor, extraction temperature is 40 DEG C, and extracting pressure is 45Mpa, and squalane is as entrainment agent, and the addition of squalane is the 8%(mass ratio of extraction kettle miospore opaque amount), the flow control of CO2 at 200L/h, extraction time 2.5h; Extract is purified through the first separating still and the second separating still successively, the separating pressure 10MPa in the first separating still, temperature 35 DEG C, and in the second separating still, separating pressure is 8MPa, and temperature is 30 DEG C; From the second separating still extract out, be Ganoderma spore oil.Prepared spore oil is transparent homogeneous, directly can add in cosmetic formulations and use.Ganoderma spore oil extraction yield is 36.4%, and detect Ganoderma powder sporoderm-broken rate is 99.2%, total triterpene contents is 4.0%.
Claims (1)
1. a preparation method for Ganoderma spore oil, is characterized in that adopting following steps:
A: first Ganoderma spore powder is dried in 40-45 DEG C of baking oven, meal pulverized to obtain by pulverizer, the ratio of meal and dehydrated alcohol liquor ratio 1:5-10 is according to quantity mixed, broken wall treatment is carried out by high pressure homogenizer under normal temperature, 70 ~ 150Mpa pressure, then by the lyophilize in Freeze Drying Equipment of gained mixed solution, Ganoderma spore powder is obtained;
B: mixed with the dextrin of 5%-8% by Ganoderma spore powder, adopts nodulizer dry method under 5 Mpa to be pressed into 20-50 object particle;
C: by the particle prepared by step B, loads CO
2in supercritical extraction reactor, at CO
2the entrance and exit of supercritical extraction reactor arranges filter paper or absorbent cotton, stops particle when extracting to pass CO
2the screen plate of supercritical extraction reactor, extraction temperature is 40 ~ 50 DEG C, and extracting pressure is 30 ~ 45Mpa, and squalane is as entrainment agent, and the addition of squalane is 5 ~ 10%, CO of extraction kettle miospore opaque amount
2flow control at 200 ~ 400L/h, extraction time 2 ~ 3h; Extract is purified through the first separating still and the second separating still successively, the separating pressure 8-10MPa in the first separating still, temperature 30-40 DEG C, separating pressure in second separating still is 5-8MPa, temperature is 20 ~ 30 DEG C, from the second separating still extract out, is Ganoderma spore oil.
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CN104274498B (en) * | 2014-09-18 | 2018-05-15 | 开平健之源保健食品有限公司 | A kind of high efficiency anti-tumor Ganodenna Lucidum P.E and preparation method thereof |
CN104531341A (en) * | 2014-12-18 | 2015-04-22 | 贵州航天乌江机电设备有限责任公司 | Process for extracting ganoderma lucidum spore oil through supercritical method |
CN105853286A (en) * | 2016-04-29 | 2016-08-17 | 山东复大生物科技有限公司 | Skin care product containing ganoderma lucidum spore oil and preparation method for ganoderma lucidum spores oil of skin care product |
CN109054992A (en) * | 2018-09-04 | 2018-12-21 | 尤建伟 | A method of extracting Seabuckthorm Seed Oil |
CN113150867B (en) * | 2020-12-01 | 2023-05-12 | 中科健康产业集团股份有限公司 | Preparation method of ganoderma lucidum extract oil rich in ganoderma lucidum triterpenes |
CN113150872A (en) * | 2021-05-07 | 2021-07-23 | 四川省运好农业开发有限公司 | Comprehensive-nutrition peony essential oil refining method |
CN114736731A (en) * | 2022-04-27 | 2022-07-12 | 山东芝人堂药业有限公司 | Supercritical CO2 process for extracting ganoderma lucidum spore oil |
CN115011407A (en) * | 2022-06-24 | 2022-09-06 | 广东钰禾生物科技有限公司 | Method for supercritical extraction of ganoderma lucidum spore oil and application of ganoderma lucidum spore oil |
CN115216361A (en) * | 2022-08-12 | 2022-10-21 | 武夷山元生泰生物科技有限公司 | Preparation method of ganoderma lucidum spore oil |
CN117324072A (en) * | 2023-10-26 | 2024-01-02 | 南京理工大学 | Spore powder low-temperature double-helix wall breaking device and continuous shearing wall breaking method |
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