CN110037258A - A kind of anti-sea-buckthorn compound superfine powder and its preparation method for being mutated, pressing down cancer and cancer cell specific induction of apoptosis - Google Patents

A kind of anti-sea-buckthorn compound superfine powder and its preparation method for being mutated, pressing down cancer and cancer cell specific induction of apoptosis Download PDF

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CN110037258A
CN110037258A CN201910298295.8A CN201910298295A CN110037258A CN 110037258 A CN110037258 A CN 110037258A CN 201910298295 A CN201910298295 A CN 201910298295A CN 110037258 A CN110037258 A CN 110037258A
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extract
sea
ursolic acid
cancer
extracting solution
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邹元生
谭志超
王辉斌
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Beijing Powdery Health Industry Co Ltd
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Beijing Powdery Health Industry Co Ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L19/00Products from fruits or vegetables; Preparation or treatment thereof
    • A23L19/01Instant products; Powders; Flakes; Granules
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L19/00Products from fruits or vegetables; Preparation or treatment thereof
    • A23L19/09Mashed or comminuted products, e.g. pulp, purée, sauce, or products made therefrom, e.g. snacks
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/33Heterocyclic compounds
    • A61K31/335Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
    • A61K31/35Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
    • A61K31/352Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline 
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/56Compounds containing cyclopenta[a]hydrophenanthrene ring systems; Derivatives thereof, e.g. steroids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/06Fungi, e.g. yeasts
    • A61K36/07Basidiomycota, e.g. Cryptococcus
    • A61K36/076Poria
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P35/00Antineoplastic agents
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

Abstract

The invention discloses the sea-buckthorn compound superfine powders and its preparation method of a kind of anti-mutation, suppression cancer and cancer cell specific induction of apoptosis, the raw material for preparing the sea-buckthorn compound superfine powder includes seabuckthorn seeds procyanidin extract, seabuckthorn fruit peel ursolic acid extract, Ilex kudingcha C.J.Tseng old leaf ursolic acid extract and fuling peel triterpene extract, wherein main active of the seabuckthorn seeds procyanidin extract as the sea-buckthorn compound superfine powder, with extremely strong antioxidant activity, free radical can be effectively removed;Ursolic acid have extensive biological effect, it is outstanding effect be it is antitumor, to it is a variety of it is carcinogenic, promote cancer objects have resistant function, have obvious cytotoxicity to a variety of cancer cells;Fuling peel triterpene extract has obvious anti-oxidant, anti-tumor activity;By the compounding of several substances, active ingredient group is formed, common synergistic effect plays the role of more effectively anti-mutation, suppression cancer and cancer cell specific induction of apoptosis.

Description

It is a kind of it is anti-mutation, suppression cancer and cancer cell specific induction of apoptosis sea-buckthorn compound superfine powder and Its preparation method
Technical field
The invention belongs to field of functional food, in particular to the sand of a kind of anti-mutation, suppression cancer and cancer cell specific induction of apoptosis Spine compound superfine powder and its preparation method.
Background technique
Cancer is to endanger the most important chronic disease of national health, has the spy of high sick hair rate, high mortality, low survival rate Point.As soon as average minute clock has 8 people to be diagnosed as cancer, has 5 currently, the whole nation is diagnosed as cancer more than ten thousand people daily Individual is dead because of cancer.The cancer neopathy case in the whole nation accounts for 4 one-tenth of the whole world.Crowd's cancer morbidity quickly increases within 30 years old or more Height, into the cancer high-incidence season, disease incidence fast lifting after 40 years old peaks for 80 years old.Nearly ten years, cancer morbidity is annual Increase about 4%, it is contemplated that arrive the year two thousand twenty, the year morbidity sum of cancer is up to 6,000,000 people or more, and annual cancer mortality sum also will Up to more than 3,000,000 people.
Gene mutation, immunologic escape are that most crucial factor occurs for cancer.Cancer develops into carcinoma in situ from normal cell and needs Take 10 ~ 30 years.Studies have shown that precancerous lesion is usually irreversible, therefore, capturing cancer should be since prevention.For this purpose, seeking It looks for safety and dietary product, health care product or the drug occurred with pre- anti-cancer is a urgent problem to be solved.
Summary of the invention
To solve the above problems, the object of the present invention is to provide the sand of a kind of anti-mutation, suppression cancer and cancer cell specific induction of apoptosis Spine compound superfine powder and its preparation method.By the compounding of several substances, active ingredient group is formed, common synergistic effect plays more The effect of effective anti-mutation, suppression cancer and cancer cell specific induction of apoptosis.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of anti-sea-buckthorn compound superfine powder for being mutated, pressing down cancer and cancer cell specific induction of apoptosis, prepares the sea-buckthorn compound Ultramicro-powder The raw material of agent includes that seabuckthorn seeds procyanidin extract, seabuckthorn fruit peel ursolic acid extract, Ilex kudingcha C.J.Tseng old leaf ursolic acid mention Take object and fuling peel triterpene extract, the weight fraction ratio of each raw material are as follows:
Seabuckthorn seeds procyanidin extract 5 ~ 20
Seabuckthorn fruit peel ursolic acid extract 30 ~ 45
Ilex kudingcha C.J.Tseng old leaf ursolic acid extract 20 ~ 40
Fuling peel triterpene extract 20 ~ 40.
Further, the seabuckthorn seeds procyanidin extract the preparation method comprises the following steps:
Through supercritical CO2Sea-buckthorn seed cake after extracting Seabuckthorm Seed Oil is impregnated at least 1 hour with 6 ~ 15 times of 40% ~ 80% ethyl alcohol, 0.2h ~ 0.5h is extracted using homogenate extraction method under 15 DEG C ~ 35 DEG C normal temperature conditions, extracting solution is collected by filtration, slag is extracted and repeats to extract 2 ~ 3 times, obtained extracting solution is repeatedly extracted in merging, then uses low-temperature negative-pressure closed loop thermo-compression evaporation enrichment facility, recycles ethyl alcohol, And concentrated extracting solution is greater than 45% concentrate to soluble solid, concentrate is dry using low-temperature negative-pressure belt drying unit, Obtain seabuckthorn seeds procyanidin extract coarse powder.
Further, the seabuckthorn fruit peel ursolic acid extract the preparation method comprises the following steps:
Seabuckthorn fruit peel is impregnated at least 1 hour with 6 ~ 15 times of 60% ~ 85% ethyl alcohol, using flash under 15 DEG C ~ 35 DEG C normal temperature conditions Extraction method extracts 0.2h ~ 0.5h, and extracting solution is collected by filtration, and extracts slag and repeats to extract 2 ~ 3 times, obtained extraction is repeatedly extracted in merging Liquid, then low-temperature negative-pressure closed loop thermo-compression evaporation enrichment facility is used, ethyl alcohol is recycled, and concentrated extracting solution is big to soluble solid In 40% concentrate, concentrate is dry using low-temperature negative-pressure belt drying unit, and it is thick to obtain seabuckthorn fruit peel ursolic acid extract Powder.
Further, the Ilex kudingcha C.J.Tseng old leaf ursolic acid extract the preparation method comprises the following steps:
Ilex kudingcha C.J.Tseng old leaf is crushed to 10 ~ 20 mesh, is impregnated at least 1 hour with 6 ~ 15 times of 60% ~ 85% ethyl alcohol, 15 DEG C ~ 0.2h ~ 0.5h is extracted using homogenate extraction method under 35 DEG C of normal temperature conditions, extracting solution is collected by filtration, slag is extracted and repeats to extract 2 ~ 3 times, Obtained extracting solution is repeatedly extracted in merging, then uses low-temperature negative-pressure closed loop thermo-compression evaporation enrichment facility, recycles ethyl alcohol, and be concentrated Extracting solution is greater than 40% concentrate to soluble solid, and concentrate is dry using low-temperature negative-pressure belt drying unit, obtains the winter Green old leaves of Kudingcha ursolic acid extract coarse powder.
Further, the fuling peel triterpene extract the preparation method comprises the following steps:
Fuling peel is crushed to 10 ~ 20 mesh, is impregnated at least 1 hour with 6 ~ 15 times of 60% ~ 85% ethyl alcohol, in 15 DEG C ~ 35 DEG C room temperature items 0.2h ~ 0.5h is extracted using homogenate extraction method under part, extracting solution is collected by filtration, slag is extracted and repeats to extract 2 ~ 3 times, merging repeatedly mentions The extracting solution obtained, then low-temperature negative-pressure closed loop thermo-compression evaporation enrichment facility is used, ethyl alcohol is recycled, and concentrated extracting solution extremely may be used Dissolubility solid content is greater than 40% concentrate, and concentrate is dry using low-temperature negative-pressure belt drying unit, obtains fuling peel triterpene and mentions Take object coarse powder.
Further, sea buckthorn procyanidins > 2.2g, ursolic acid > 1.6g in every 100g sea-buckthorn compound superfine powder.
Further, the low-temperature negative-pressure is that temperature is lower than 50 DEG C, and pressure is higher than -0.098MPa.
The preparation method of the sea-buckthorn compound superfine powder, comprising the following steps:
By seabuckthorn seeds procyanidin extract coarse powder, seabuckthorn fruit peel ursolic acid extract coarse powder, Ilex kudingcha C.J.Tseng old leaf ursolic acid Extract coarse powder and fuling peel triterpene extract coarse powder are proportionally added in three-dimensional mixer and are uniformly mixed, then will mixing After uniform coarse powder is crushed to the Ultramicro-powder of 500 mesh or more using airslide disintegrating mill, the filling sea-buckthorn compound ultra micro at every bag of 6g Powder product.
The present invention having the beneficial effect that compared with prior art
1, the raw material of sea-buckthorn compound superfine powder of the present invention, belongs to the kind of dual-purpose of drug and food, has no toxic side effect, it is ensured that The safety of product, can take for a long time;
2, the preparation method of sea-buckthorn compound superfine powder of the present invention, using the technology of room temperature homogenate extraction, low temperature (50 DEG C with Under), negative pressure (- 0.098MPa or more) closed loop thermo-compression evaporation concentration technique, low temperature (50 DEG C or less), negative pressure (- 0.098MPa with On) belt drying technology, temperature is low, the time is short, has not only been effectively maintained the bioactivity of product, but also energy conservation and environmental protection, greatly Production cost is reduced greatly.
Specific embodiment
Embodiment 1
The sea-buckthorn compound superfine powder of a kind of anti-mutation, suppression cancer and cancer cell specific induction of apoptosis is present embodiments provided, described in preparation The raw material of sea-buckthorn compound superfine powder includes seabuckthorn seeds procyanidin extract, seabuckthorn fruit peel ursolic acid extract, Chinese ilex bitter leaves Tea old leaf ursolic acid extract and fuling peel triterpene extract, the weight of each raw material are as follows:
Seabuckthorn seeds procyanidin extract 6kg
Seabuckthorn fruit peel ursolic acid extract 40kg
Ilex kudingcha C.J.Tseng old leaf ursolic acid extract 38kg
Fuling peel triterpene extract 36kg.
The seabuckthorn seeds procyanidin extract the preparation method comprises the following steps:
Through supercritical CO2Sea-buckthorn seed cake 60kg after extracting Seabuckthorm Seed Oil is impregnated at least 1 hour with 10 times of 60% ethyl alcohol, 15 DEG C ~ 35 DEG C of normal temperature conditions under using homogenate extraction method extract 0.3h, 300 mesh are collected by filtration extracting solution, extract slag and 6 times are added again 60% ethyl alcohol, extract 0.3h using homogenate extraction method under 15 DEG C again ~ 35 DEG C normal temperature conditions, the filtering of 300 mesh is collected again extracts Liquid, merges the extracting solution extracted twice, and extracting solution uses 45 DEG C of negative pressure (- 0.098MPa or more) closed loop thermo-compression evaporations again Enrichment facility recycles ethyl alcohol, and concentrated extracting solution is greater than 40% concentrate to soluble solid, and concentrate is negative using low temperature Press belt type dryer group is dry, obtains seabuckthorn seeds procyanidin extract coarse powder 6kg.
The seabuckthorn fruit peel ursolic acid extract the preparation method comprises the following steps:
12 times of 85% ethyl alcohol of 208kg seabuckthorn fruit peel is impregnated at least 1 hour, using flash under 15 DEG C ~ 35 DEG C normal temperature conditions Extraction method extracts 0.3h, and extracting solution is collected by filtration in 300 mesh, extracts 85% ethyl alcohol that slag is added 6 times again, 15 DEG C again ~ 35 DEG C often 0.3h is extracted using homogenate extraction method under the conditions of temperature, the filtering of 300 mesh collects extracting solution again, merges the extraction extracted twice Liquid, then 45 DEG C of negative pressure (- 0.098MPa or more) closed loop thermo-compression evaporation enrichment facilities are used, recycle ethyl alcohol, and concentrated extracting solution It is greater than 40% concentrate A to soluble solid;Filter residue after extracting twice, is added 15 times of pure water, and 90 DEG C or more slightly boiled to mention After taking 1.5h, filtrate is obtained by filtration in 300 mesh, and 60 DEG C of negative pressure (- 0.098MPa or more) of the filtrate are concentrated through closed loop thermo-compression evaporation Device is concentrated into the concentrate B that soluble solids are greater than 40%, merges concentrate A and concentrate B, then below low using 50 DEG C Warm negative pressure (- 0.098MPa or more) belt drying unit is dry, obtains seabuckthorn fruit peel ursolic acid extract coarse powder 40kg.
The Ilex kudingcha C.J.Tseng old leaf ursolic acid extract the preparation method comprises the following steps:
240kg Ilex kudingcha C.J.Tseng old leaf is crushed to the coarse powder of 10 ~ 20 mesh, is impregnated at least 1 hour with 12 times of 85% ethyl alcohol, 0.3h is extracted using homogenate extraction method under 15 DEG C ~ 35 DEG C normal temperature conditions, extracting solution is collected by filtration in 300 mesh, extracts slag and 6 are added again Times 85% ethyl alcohol, extract 0.3h using homogenate extraction method under 15 DEG C again ~ 35 DEG C normal temperature conditions, the filtering of 300 mesh is collected again to be mentioned Liquid is taken, merges the extracting solution extracted twice, then using 45 DEG C of negative pressure (- 0.098MPa or more) closed loop thermo-compression evaporation concentrations Device recycles ethyl alcohol, and concentrated extracting solution is greater than 40% concentrate to soluble solid, and concentrate is below using 50 DEG C Low-temperature negative-pressure (- 0.098MPa or more) belt drying unit is dry, obtains Ilex kudingcha C.J.Tseng old leaf ursolic acid extract coarse powder 38kg。
The fuling peel triterpene extract the preparation method comprises the following steps:
255kg fuling peel is crushed to the coarse powder of 10 ~ 20 mesh, is impregnated at least 1 hour with 10 times of 85% ethyl alcohol, at 15 DEG C ~ 35 DEG C 0.3h is extracted using homogenate extraction method under normal temperature condition, extracting solution is collected by filtration, extracts 85% ethyl alcohol that slag is added 6 times again, then 0.3h is extracted using homogenate extraction method under secondary 15 DEG C ~ 35 DEG C normal temperature conditions, the filtering of 300 mesh is collected extracting solution again, merged twice Obtained extracting solution is extracted, then uses 45 DEG C of negative pressure (- 0.098MPa or more) closed loop thermo-compression evaporation enrichment facilities, recycles second Alcohol, and concentrated extracting solution is greater than 40% concentrate to soluble solid, concentrate using 50 DEG C of low-temperature negative-pressures below (- 0.098MPa or more) drying of belt drying unit, obtain fuling peel triterpene extract coarse powder 36kg.
The preparation method of the sea-buckthorn compound superfine powder, comprising the following steps:
By seabuckthorn seeds procyanidin extract coarse powder 6kg, seabuckthorn fruit peel ursolic acid extract coarse powder 40kg, Ilex kudingcha C.J.Tseng old leaf Ursolic acid extract coarse powder 38kg and fuling peel triterpene extract coarse powder 36kg is added in three-dimensional mixer and is uniformly mixed, then Uniformly mixed coarse powder is crushed to the Ultramicro-powder 120kg of 500 mesh or more using airslide disintegrating mill, it is filling at described in every bag of 6g Sea-buckthorn compound superfine powder product, 20000 bags of theoretical yield.
Through detecting, sea buckthorn procyanidins > 2.2g in every 100g sea-buckthorn compound superfine powder;Ursolic acid > 1.6g.
The taking dose and method of the sea-buckthorn compound superfine powder are as follows: 1 bag every time, 2 times a day.
Embodiment 2
The sea-buckthorn compound superfine powder of a kind of anti-mutation, suppression cancer and cancer cell specific induction of apoptosis is present embodiments provided, described in preparation The raw material of sea-buckthorn compound superfine powder includes seabuckthorn seeds procyanidin extract, seabuckthorn fruit peel ursolic acid extract, Chinese ilex bitter leaves Tea old leaf ursolic acid extract and fuling peel triterpene extract, the weight of each raw material are as follows:
Seabuckthorn seeds procyanidin extract 15kg
Seabuckthorn fruit peel ursolic acid extract 72kg
Ilex kudingcha C.J.Tseng old leaf ursolic acid extract 47kg
Fuling peel triterpene extract 46kg.
The seabuckthorn seeds procyanidin extract the preparation method comprises the following steps:
Through supercritical CO2Sea-buckthorn seed cake 145kg after extracting Seabuckthorm Seed Oil is impregnated at least 1 hour with 10 times of 60% ethyl alcohol, 0.3h is extracted using homogenate extraction method under 15 DEG C ~ 35 DEG C normal temperature conditions, extracting solution is collected by filtration in 300 mesh, extracts slag and 6 are added again Times 60% ethyl alcohol, extract 0.3h using homogenate extraction method under 15 DEG C again ~ 35 DEG C normal temperature conditions, the filtering of 300 mesh is collected again to be mentioned Liquid is taken, the extracting solution extracted twice is merged, extracting solution uses 45 DEG C of negative pressure (- 0.098MPa or more) closed loop heat pumps to steam again Enrichment facility is sent out, recycles ethyl alcohol, and concentrated extracting solution is greater than 40% concentrate to soluble solid, concentrate uses low temperature Negative pressure belt drying unit is dry, obtains seabuckthorn seeds procyanidin extract coarse powder 15kg.
The seabuckthorn fruit peel ursolic acid extract the preparation method comprises the following steps:
12 times of 85% ethyl alcohol of 522kg seabuckthorn fruit peel is impregnated at least 1 hour, using flash under 15 DEG C ~ 35 DEG C normal temperature conditions Extraction method extracts 0.3h, and extracting solution is collected by filtration in 300 mesh, extracts 85% ethyl alcohol that slag is added 6 times again, 15 DEG C again ~ 35 DEG C often 0.3h is extracted using homogenate extraction method under the conditions of temperature, the filtering of 300 mesh collects extracting solution again, merges the extraction extracted twice Liquid, then 45 DEG C of negative pressure (- 0.098MPa or more) closed loop thermo-compression evaporation enrichment facilities are used, recycle ethyl alcohol, and concentrated extracting solution It is greater than 40% concentrate A to soluble solid;Filter residue after extracting twice, is added 15 times of pure water, and 90 DEG C or more slightly boiled to mention After taking 1.5h, filtrate is obtained by filtration in 300 mesh, and 60 DEG C of negative pressure (- 0.098MPa or more) of the filtrate are concentrated through closed loop thermo-compression evaporation Device is concentrated into the concentrate B that soluble solids are greater than 40%, merges concentrate A and concentrate B, then below low using 50 DEG C Warm negative pressure (- 0.098MPa or more) belt drying unit is dry, obtains seabuckthorn fruit peel ursolic acid extract coarse powder 72kg.
The Ilex kudingcha C.J.Tseng old leaf ursolic acid extract the preparation method comprises the following steps:
288kg Ilex kudingcha C.J.Tseng old leaf is crushed to the coarse powder of 10 ~ 20 mesh, is impregnated at least 1 hour with 12 times of 85% ethyl alcohol, 0.3h is extracted using homogenate extraction method under 15 DEG C ~ 35 DEG C normal temperature conditions, extracting solution is collected by filtration in 300 mesh, extracts slag and 6 are added again Times 85% ethyl alcohol, extract 0.3h using homogenate extraction method under 15 DEG C again ~ 35 DEG C normal temperature conditions, the filtering of 300 mesh is collected again to be mentioned Liquid is taken, merges the extracting solution extracted twice, then using 45 DEG C of negative pressure (- 0.098MPa or more) closed loop thermo-compression evaporation concentrations Device recycles ethyl alcohol, and concentrated extracting solution is greater than 40% concentrate to soluble solid, and concentrate is below using 50 DEG C Low-temperature negative-pressure (- 0.098MPa or more) belt drying unit is dry, obtains Ilex kudingcha C.J.Tseng old leaf ursolic acid extract coarse powder 47kg。
The fuling peel triterpene extract the preparation method comprises the following steps:
280kg fuling peel is crushed to the coarse powder of 10 ~ 20 mesh, is impregnated at least 1 hour with 10 times of 85% ethyl alcohol, at 15 DEG C ~ 35 DEG C 0.3h is extracted using homogenate extraction method under normal temperature condition, extracting solution is collected by filtration, extracts 85% ethyl alcohol that slag is added 6 times again, then 0.3h is extracted using homogenate extraction method under secondary 15 DEG C ~ 35 DEG C normal temperature conditions, the filtering of 300 mesh is collected extracting solution again, merged twice Obtained extracting solution is extracted, then uses 45 DEG C of negative pressure (- 0.098MPa or more) closed loop thermo-compression evaporation enrichment facilities, recycles second Alcohol, and concentrated extracting solution is greater than 40% concentrate to soluble solid, concentrate using 50 DEG C of low-temperature negative-pressures below (- 0.098MPa or more) drying of belt drying unit, obtain fuling peel triterpene extract coarse powder 46kg.
The preparation method of the sea-buckthorn compound superfine powder, comprising the following steps:
Seabuckthorn seeds procyanidin extract coarse powder 15kg, seabuckthorn fruit peel ursolic acid extract coarse powder 72kg, Ilex kudingcha C.J.Tseng is old Leaf ursolic acid extract coarse powder 47kg and fuling peel triterpene extract coarse powder 46kg is added in three-dimensional mixer and is uniformly mixed, Uniformly mixed coarse powder is crushed to the Ultramicro-powder 180kg of 500 mesh or more, the filling institute at every bag of 6g using airslide disintegrating mill again State sea-buckthorn compound superfine powder product, 30000 bags of theoretical yield.
Through detecting, sea buckthorn procyanidins > 2.2g in every 100g sea-buckthorn compound superfine powder;Ursolic acid > 1.6g.
The taking dose and method of the sea-buckthorn compound superfine powder are as follows: 1 bag every time, 2 times a day.

Claims (9)

1. the sea-buckthorn compound superfine powder of a kind of anti-mutation, suppression cancer and cancer cell specific induction of apoptosis, which is characterized in that prepare the sand The raw material of spine compound superfine powder includes seabuckthorn seeds procyanidin extract, seabuckthorn fruit peel ursolic acid extract, Ilex kudingcha C.J.Tseng Old leaf ursolic acid extract and fuling peel triterpene extract, the weight fraction ratio of each raw material are as follows:
Seabuckthorn seeds procyanidin extract 5 ~ 20
Seabuckthorn fruit peel ursolic acid extract 30 ~ 45
Ilex kudingcha C.J.Tseng old leaf ursolic acid extract 20 ~ 40
Fuling peel triterpene extract 20 ~ 40.
2. the sea-buckthorn compound superfine powder of mutation according to claim 1, suppression cancer and cancer cell specific induction of apoptosis, feature exist In the weight fraction ratio of each raw material are as follows:
Seabuckthorn seeds procyanidin extract 10 ~ 15
Seabuckthorn fruit peel ursolic acid extract 20 ~ 35
Ilex kudingcha C.J.Tseng old leaf ursolic acid extract 10 ~ 30
Fuling peel triterpene extract 10 ~ 30.
3. the sea-buckthorn compound superfine powder of mutation according to claim 1, suppression cancer and cancer cell specific induction of apoptosis, feature exist In, the seabuckthorn seeds procyanidin extract the preparation method comprises the following steps:
Through supercritical CO2Sea-buckthorn seed cake after extracting Seabuckthorm Seed Oil is impregnated at least 1 hour with 6 ~ 15 times of 40% ~ 80% ethyl alcohol, 0.2h ~ 0.5h is extracted using homogenate extraction method under 15 DEG C ~ 35 DEG C normal temperature conditions, extracting solution is collected by filtration, slag is extracted and repeats to extract 2 ~ 3 times, obtained extracting solution is repeatedly extracted in merging, then uses low-temperature negative-pressure closed loop thermo-compression evaporation enrichment facility, recycles ethyl alcohol, And concentrated extracting solution is greater than 40% concentrate to soluble solid, concentrate is dry using low-temperature negative-pressure belt drying unit, Obtain seabuckthorn seeds procyanidin extract coarse powder.
4. the sea-buckthorn compound superfine powder of mutation according to claim 1, suppression cancer and cancer cell specific induction of apoptosis, feature exist In, the seabuckthorn fruit peel ursolic acid extract the preparation method comprises the following steps:
Seabuckthorn fruit peel is impregnated at least 1 hour with 6 ~ 15 times of 60% ~ 85% ethyl alcohol, using flash under 15 DEG C ~ 35 DEG C normal temperature conditions Extraction method extracts 0.2h ~ 0.5h, and extracting solution is collected by filtration, and extracts slag and repeats to extract 2 ~ 3 times, obtained extraction is repeatedly extracted in merging Liquid, then low-temperature negative-pressure closed loop thermo-compression evaporation enrichment facility is used, ethyl alcohol is recycled, and concentrated extracting solution is big to soluble solid In 40% concentrate, concentrate is dry using low-temperature negative-pressure belt drying unit, and it is thick to obtain seabuckthorn fruit peel ursolic acid extract Powder.
5. the sea-buckthorn compound superfine powder of mutation according to claim 1, suppression cancer and cancer cell specific induction of apoptosis, feature exist In, the Ilex kudingcha C.J.Tseng old leaf ursolic acid extract the preparation method comprises the following steps:
Ilex kudingcha C.J.Tseng old leaf is crushed to 10 ~ 20 mesh, is impregnated at least 1 hour with 6 ~ 15 times of 60% ~ 85% ethyl alcohol, 15 DEG C ~ 0.2h ~ 0.5h is extracted using homogenate extraction method under 35 DEG C of normal temperature conditions, extracting solution is collected by filtration, slag is extracted and repeats to extract 2 ~ 3 times, Obtained extracting solution is repeatedly extracted in merging, then uses low-temperature negative-pressure closed loop thermo-compression evaporation enrichment facility, recycles ethyl alcohol, and be concentrated Extracting solution is greater than 40% concentrate to soluble solid, and concentrate is dry using low-temperature negative-pressure belt drying unit, obtains the winter Green old leaves of Kudingcha ursolic acid extract coarse powder.
6. the sea-buckthorn compound superfine powder of mutation according to claim 1, suppression cancer and cancer cell specific induction of apoptosis, feature exist In, the fuling peel triterpene extract the preparation method comprises the following steps:
Fuling peel is crushed to 10 ~ 20 mesh, is impregnated at least 1 hour with 6 ~ 15 times of 60% ~ 85% ethyl alcohol, in 15 DEG C ~ 35 DEG C room temperature items 0.2h ~ 0.5h is extracted using homogenate extraction method under part, extracting solution is collected by filtration, slag is extracted and repeats to extract 2 ~ 3 times, merging repeatedly mentions The extracting solution obtained, then low-temperature negative-pressure closed loop thermo-compression evaporation enrichment facility is used, ethyl alcohol is recycled, and concentrated extracting solution extremely may be used Dissolubility solid content is greater than 40% concentrate, and concentrate is dry using low-temperature negative-pressure belt drying unit, obtains fuling peel triterpene and mentions Take object coarse powder.
7. the sea-buckthorn compound Ultramicro-powder of anti-mutation according to claim 1-6, suppression cancer and cancer cell specific induction of apoptosis Agent, which is characterized in that sea buckthorn procyanidins > 2.2g, ursolic acid > 1.6g in every 100g sea-buckthorn compound superfine powder.
8. according to the sea-buckthorn compound Ultramicro-powder of the described in any item anti-mutation of claim 3-6, suppression cancer and cancer cell specific induction of apoptosis Agent, which is characterized in that the low-temperature negative-pressure is that temperature is lower than 50 DEG C, and pressure is higher than -0.098MPa.
9. a kind of preparation method of the sea-buckthorn compound superfine powder as described in claim any one of 1-8, which is characterized in that the system Preparation Method the following steps are included:
By seabuckthorn seeds procyanidin extract coarse powder, seabuckthorn fruit peel ursolic acid extract coarse powder, Ilex kudingcha C.J.Tseng old leaf ursolic acid Extract coarse powder and fuling peel triterpene extract coarse powder are proportionally added in three-dimensional mixer and are uniformly mixed, then will mixing After uniform coarse powder is crushed to the Ultramicro-powder of 500 mesh or more using airslide disintegrating mill, the filling sea-buckthorn compound ultra micro at every bag of 6g Powder product.
CN201910298295.8A 2019-04-15 2019-04-15 A kind of anti-sea-buckthorn compound superfine powder and its preparation method for being mutated, pressing down cancer and cancer cell specific induction of apoptosis Pending CN110037258A (en)

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