CN104083337A - Preparation method of sulforaphane capsule - Google Patents
Preparation method of sulforaphane capsule Download PDFInfo
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- CN104083337A CN104083337A CN201410215852.2A CN201410215852A CN104083337A CN 104083337 A CN104083337 A CN 104083337A CN 201410215852 A CN201410215852 A CN 201410215852A CN 104083337 A CN104083337 A CN 104083337A
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Abstract
The invention discloses a preparation method of a sulforaphane capsule. The method comprises the following steps: 1, mixing crude sulforaphane powder with auxiliary materials, and drying the above obtained mixture; 2, grinding the dried sulforaphane and auxiliary material mixture until the diameter of obtained particles is below 100nm; and 4, adding the ground sulforaphane and auxiliary material mixture into a capsule. The method disclosed in the invention overcomes the problems of insufficient fragmentation and inconvenient human body absorption of effective components of capsules produced through present production methods, has a simple production process, and is suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of processing of health product and the method for production technology thereof of medicine-food two-purpose, the capsule preparation method thereof that specifically a kind of Sulforaphane is raw material.
Background technology
Sulforaphane, claims again raphanin, is a kind of efficient chemical functional material, is the strongest anticancer component of finding in vegetable up to now.Sulforaphane is glucose radish seed glycoside (glucosinolate, be a kind of of thioglycoside) isothiocyanate (Isothiocyanates that produces through myrosinase (Myrosinase) enzymolysis or acid hydrolysis, be called for short ITCs), in Radix Raphani, find and gain the name, soluble in water, relative molecular weight is 177.3, and molecular formula is C6H11S2NO, and the structural formula of Sulforaphane is shown in formula 1.
Formula 1 sulforaphen chemical structural formula
Sulforaphane is the most significant isothiocyanic acid salt compounds of antioxidation, anti-cancer, active anticancer of finding at present.Oneself is through clearer and more definite now, and Sulforaphane can be prevented Normocellular canceration.But the inhibition cancerous tumor cell proliferative effect of the most attracting or Sulforaphane compound and analog thereof.The Sulforaphane of having reported at present can have prophylactic activity to hepatocarcinoma, pulmonary carcinoma, carcinoma of prostate, breast carcinoma, colon and rectum carcinoma, the esophageal carcinoma, front gastric cancer, bladder cancer, cancer of pancreas, and also has certain antiinflammatory action.
Document and patent report the method such as the alcohol extraction of Sulforaphane and water extraction, then by the mode of macroporous resin, silica gel and C18 column chromatography, carry out purification.Its document and Patent are as follows:
< < method (CN101143842) > > who extracts sulforaphen, < < broccoli seed extractive and preparation method thereof (CN101229211) > >, preparation method (CN1982294) the > > of a < < Sulforaphane, extracting method (CN101544995) the > > of a < < sulforaphen, extraction and the purification process of effective active composition sulforaphen in broccoli seed all disclosed.The problem that these methods exist has: in purge process, all adopt silica gel column chromatography, with C18 preparative hplc or gel column, carry out purification Sulforaphane again, in silicagel column developing solvent, use poisonous organic solvent eluting, also there is inflammable and explosive problem in production process, add the defects such as column chromatography material regeneration is more difficult, cause above-mentioned patent to be only suitable for small lot and laboratory is prepared use, be unsuitable for suitability for industrialized production.
The method for extraction and purification of a < < high-purity sulforaphen (CN 102898341) > > discloses and from broccoli seed, after ultrasonic alcohol extraction, has adopted macroporous resin to carry out purification, with alumina column chromatography, then adopt polar reagent extraction mode purification to obtain highly purified Sulforaphane.In patent, adopt polar reagent extraction very easily to cause organic reagent residual, and processing step is complicated, is difficult for realizing suitability for industrialized production.
Patent < < method (CN 103436565) > > who extracts sulforaphen from Caulis et Folium Brassicae capitatae discloses a kind of method of extracting sulforaphen from Caulis et Folium Brassicae capitatae vegetable, process using first dry plant, add again enzyme to be hydrolyzed, adopt the mode of organic reagent extraction, process big energy-consuming, process is complicated, in Caulis et Folium Brassicae capitatae, sulforaphen content is lower, add enzyme hydrolysis not thorough, be difficult for carrying out large-scale industrial production.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of Sulforaphane capsule, to overcome the problem that the capsule effective ingredient fragmentation of existing production method is insufficient, be not easy to absorption of human body, is suitable for suitability for industrialized production.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of preparation method of Sulforaphane capsule is provided, and it comprises the following steps:
(1) Sulforaphane coarse powder and adjuvant are mixed together and are dried;
(2) mixture of dried Sulforaphane and adjuvant is ground to the microgranule below diameter 100nm;
(3) during the mixture of the Sulforaphane after grinding and adjuvant is incapsulated.
In a preferred embodiment of the present invention, the mass percentage content of described Sulforaphane coarse powder in described mixture is 0.5% ~ 5%.
In a preferred embodiment of the present invention, described step (1) comprises the following steps:
(a) get broccoli seed through pulverizing, add water, the hydrolysis that heats up, obtains hydrolysis mixed liquor;
(b) in hydrolysis mixed liquor, add water or buffer, regulate the pH value of mixed liquor, Sulforaphane is extracted in hydrolysis, obtains extracting solution;
(c) extracting solution is heated up deactivation hydrolytic enzyme, obtains Sulforaphane extracting solution;
(d) the Sulforaphane phase in concentrated Sulforaphane extracting solution, and to Sulforaphane phase drying under reduced pressure, makes Sulforaphane mass percentage content and is 5% ~ 20% Powdered Sulforaphane coarse powder.
In a preferred embodiment of the present invention, further comprising the steps of: Sulforaphane extracting solution is concentrated through macroporous resin adsorption, and the organic reagent eluting that then working concentration increases gradually respectively, collects and be rich in Sulforaphane phase; Add adjuvant dry.
In a preferred embodiment of the present invention, described adjuvant is a kind of or its combination in resistant dextrin, starch, sodium carboxymethyl cellulose, microcrystalline Cellulose.
In a preferred embodiment of the present invention, the broccoli seed described in step (a) is through being crushed to 10 ~ 50 orders; The described amount that adds water is equivalent to 2 ~ 5 times of amounts of described dry broccoli seed quality; Described hydrolysis temperature is 20 ~ 50 ℃, and hydrolysis time is 5 ~ 20 h.
In a preferred embodiment of the present invention, the quality that adds water described in step (b) is 10 ~ 25 times of described dry broccoli seed quality; The reagent that the pH value of described adjusting mixed liquor is used or buffer are a kind of in citric acid-sodium hydroxide-hydrochloride buffer, hydrochloric acid, sulphuric acid; Regulator solution pH value is 2 ~ 4; Described hydrolysis temperature is 20 ~ 50 ℃; Described extracting mode is for to stir extraction to regulator solution, and the rotating speed of agitating device used is 10 ~ 100 rmp, and extraction time is 5 ~ 18 h.
In a preferred embodiment of the present invention, described in step (c), extracting solution temperature is warming up to 70 ~ 80 ℃ of deactivations, and inactivation time is 5 ~ 15min.
In a preferred embodiment of the present invention, the organic reagent that described concentration increases is gradually alcoholic solution, and the concentration of described alcoholic solution is respectively 10%, 60%, 90%; Describedly be rich in the ethanol phase that Sulforaphane organic facies is concentration 60%.
In a preferred embodiment of the present invention, described adjuvant is a kind of in resistant dextrin, starch, sodium carboxymethyl cellulose, microcrystalline Cellulose.
The invention has the beneficial effects as follows: the problem that the Sulforaphane capsule effective ingredient fragmentation that overcome existing production method is insufficient, be not easy to absorption of human body, production technology is simple, is suitable for suitability for industrialized production.
The specific embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making all other embodiment that obtain under creative work prerequisite, belong to the scope of protection of the invention.
The embodiment of the present invention one:
Take dry broccoli seed 200g, after pulverizer is pulverized, cross 10 mesh sieves.Powder after pulverizing is poured in 5000 L beakers, then added 400 mL pure water, beaker is placed in water-bath, be warming up to 20 ℃, 50 rpm rotating speeds stir, hydrolysis 15 h.After hydrolysis finishes, to adding the pre-configured pH of 3000 mL in beaker, be 2.0 citric acids-sodium hydroxide-hydrochloride buffer, 100 rpm rotating speeds stir 18 h and extract.
After extraction finishes, mixed liquor is adopted to vacuum filtration, get liquid phase, obtain extracting solution, extracting solution is poured in 5000 mL beakers, beaker is inserted in water-bath, be warming up to 70 ℃, insulation 15min, is then cooled to 20 ℃.Extracting solution is adsorbed through macroporous resin D101B, then with the ethanol elution of 1000 mL concentration 10%, remove impurity, then use the ethanol elution Sulforaphane of 2000 mL concentration 60%, collect this Sulforaphane phase, finally use the alcohol flushing macroporous resin pillar of 1000 mL concentration 90%, treat to use next time.By the Sulforaphane of concentration 60% under-0.1MPa vacuum 45 ℃ reclaim ethanol, be dried to extractum shape, then add resistant dextrin 3 g, 50 ℃ of dry 5 h of-0.1MPa, the dry powder that to obtain 8 .3g Sulforaphane content be 9.1%.In dry powder, add 67g resistant dextrin, through nano level pulverizer, be crushed to 100 nm particle powders, this powder tank is dressed up to 300 of capsules.
The embodiment of the present invention two:
Take dry broccoli seed 200g, after destructor is pulverized, cross 50 mesh sieves.Powder after pulverizing is poured in 5000 L beakers, then added 1000mL pure water, beaker is placed in water-bath, be warming up to 50 ℃, 50 rpm stir, hydrolysis 8h.After hydrolysis finishes, in beaker, add 5000mL, the hydrochloric acid conditioning solution pH that uses pre-configured 2moL/L is that 4.0,100 rpm rotating speeds stir 5h extraction.
After extraction finishes, mixed liquor is adopted to vacuum filtration, get liquid phase, obtain extracting solution, extracting solution is poured in 5000 mL beakers, beaker is inserted in water-bath, be warming up to 80 ℃, insulation 5min, is then cooled to 20 ℃.Extracting solution is adsorbed through macroporous resin SP850, with the ethanol that 1000mL concentration is 10%, remove impurity, the ethanol elution Sulforaphane that is then 60% by 2000mL concentration, collects this Sulforaphane phase, the alcohol flushing macroporous resin pillar that is finally 90% by 1000mL concentration, treats to use next time.By the Sulforaphane of concentration 60% under-0.07MPa vacuum 70 ℃ reclaim ethanol, be dried to extractum shape, then add resistant dextrin 3 g, 20 ℃ of dry 15 h of-0.07MPa, the dry powder that to obtain 9 .3g Sulforaphane content be 8.3%.In dry powder, add 6g starch, through pulverizer, be crushed to 100 nm particle powders, this powder tank is dressed up to 60 of capsules.
The embodiment of the present invention three:
Take broccoli seed 200g, after destructor is pulverized, cross 24 mesh sieves.Powder after pulverizing is poured in 5000 L beakers, then added 400mL pure water, beaker is placed in water-bath, be warming up to 20 ℃, 50 rpm rotating speeds stir, hydrolysis 15 h.After hydrolysis finishes, to adding the pre-configured pH of 2600 mL in beaker, be 2.0 citric acids-sodium hydroxide-hydrochloride buffer, 100 rpm rotating speeds stir 18h and extract.
After extraction finishes, mixed liquor is adopted to vacuum filtration, get liquid phase, obtain extracting solution, extracting solution is poured in 5000mL beaker, beaker is inserted in water-bath, be warming up to 70 ℃, insulation 15min, is then cooled to 20 ℃.Extracting solution is adsorbed through macroporous resin H-60, with the ethanol that 1000mL concentration is 10%, remove impurity, the ethanol elution Sulforaphane that is then 60% by 2000mL concentration, collects this Sulforaphane phase, the alcohol flushing macroporous resin pillar that is finally 90% by 1000mL concentration, treats to use next time.By the Sulforaphane of concentration 60% under-0.1MPa vacuum 45 ℃ reclaim ethanol, be dried to extractum shape, then add microcrystalline Cellulose 3g, 50 ℃ of dry 5h of-0.1MPa, obtain the dry powder that 6.3g Sulforaphane content is 7.9%.In dry powder, add starch 5g and sodium carboxymethyl cellulose, through pulverizer, be crushed to 100 nm particle powders, this powder tank is dressed up to 60 of capsules.
The beneficial effect of the preparation method of Sulforaphane capsule of the present invention is:
The present invention has overcome the problem that the Sulforaphane capsule effective ingredient fragmentation of existing production method is insufficient, be not easy to absorption of human body, and production technology is simple, is suitable for suitability for industrialized production.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes description of the present invention to do; or be directly or indirectly used in other relevant technical field, be all in like manner included in scope of patent protection of the present invention.
Claims (10)
1. a preparation method for Sulforaphane capsule, is characterized in that, comprises the following steps:
(1) Sulforaphane coarse powder and adjuvant are mixed together and are dried;
(2) mixture of dried Sulforaphane and adjuvant is ground to the microgranule below diameter 100nm;
(3) during the mixture of the Sulforaphane after grinding and adjuvant is incapsulated.
2. the preparation method of Sulforaphane capsule according to claim 1, is characterized in that, the mass percentage content of described Sulforaphane coarse powder in described mixture is 0.5% ~ 5%.
3. the preparation method of Sulforaphane capsule according to claim 1, is characterized in that, step (1) comprises the following steps:
(a) get broccoli seed through pulverizing, add water, the hydrolysis that heats up, obtains hydrolysis mixed liquor;
(b) in hydrolysis mixed liquor, add water or buffer, regulate the pH value of mixed liquor, Sulforaphane is extracted in hydrolysis, obtains extracting solution;
(c) extracting solution is heated up deactivation hydrolytic enzyme, obtains Sulforaphane extracting solution;
(d) the Sulforaphane phase in concentrated Sulforaphane extracting solution, and to Sulforaphane phase drying under reduced pressure, makes Sulforaphane mass percentage content and is 5% ~ 20% Powdered Sulforaphane coarse powder.
4. the preparation method of Sulforaphane capsule according to claim 3, it is characterized in that, comprise the following steps: Sulforaphane extracting solution is concentrated through macroporous resin adsorption, and the organic reagent eluting that then working concentration increases gradually respectively, collects and be rich in Sulforaphane phase; Add adjuvant dry.
5. the preparation method of Sulforaphane capsule according to claim 1, is characterized in that, described adjuvant is a kind of or its combination in resistant dextrin, starch, sodium carboxymethyl cellulose, microcrystalline Cellulose.
6. the preparation method of Sulforaphane capsule according to claim 3, is characterized in that, the broccoli seed described in step (a) is through being crushed to 10 ~ 50 orders; The described amount that adds water is equivalent to 2 ~ 5 times of amounts of described dry broccoli seed quality; Described hydrolysis temperature is 20 ~ 50 ℃, and hydrolysis time is 5 ~ 20 h.
7. the preparation method of Sulforaphane capsule according to claim 3, is characterized in that, the quality that adds water described in step (b) is 10 ~ 25 times of described dry broccoli seed quality; The reagent that the pH value of described adjusting mixed liquor is used or buffer are a kind of in citric acid-sodium hydroxide-hydrochloride buffer, hydrochloric acid, sulphuric acid; Regulator solution pH value is 2 ~ 4; Described hydrolysis temperature is 20 ~ 50 ℃; Described extracting mode is for to stir extraction to regulator solution, and the rotating speed of agitating device used is 10 ~ 100 rmp, and extraction time is 5 ~ 18 h.
8. the preparation method of Sulforaphane capsule according to claim 3, is characterized in that, described in step (c), extracting solution temperature is warming up to 70 ~ 80 ℃ of deactivations, and inactivation time is 5 ~ 15min.
9. the preparation method of Sulforaphane capsule according to claim 4, is characterized in that, the organic reagent that described concentration increases is gradually alcoholic solution, and the concentration of described alcoholic solution is respectively 10%, 60%, 90%; Describedly be rich in the ethanol phase that Sulforaphane organic facies is concentration 60%.
10. the preparation method of Sulforaphane capsule according to claim 4, is characterized in that, described adjuvant is a kind of in resistant dextrin, starch, sodium carboxymethyl cellulose, microcrystalline Cellulose.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410215852.2A CN104083337A (en) | 2014-05-22 | 2014-05-22 | Preparation method of sulforaphane capsule |
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| CN201410215852.2A CN104083337A (en) | 2014-05-22 | 2014-05-22 | Preparation method of sulforaphane capsule |
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| CN104083337A true CN104083337A (en) | 2014-10-08 |
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| CN201410215852.2A Pending CN104083337A (en) | 2014-05-22 | 2014-05-22 | Preparation method of sulforaphane capsule |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023036250A1 (en) * | 2021-09-08 | 2023-03-16 | 北京化工大学 | Drug used for treating prostatitis or prostatic hyperplasia |
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| CN102234245A (en) * | 2011-05-06 | 2011-11-09 | 南京泽朗医药科技有限公司 | Method for preparing sulforaphane |
| CN102949430A (en) * | 2012-11-01 | 2013-03-06 | 上海中海龙高新技术研究院 | Maca capsule and preparation method thereof |
| US20130323225A1 (en) * | 2012-06-05 | 2013-12-05 | Jarrow Formulas, Inc. | Broccoli Based Nutritional Supplements |
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2014
- 2014-05-22 CN CN201410215852.2A patent/CN104083337A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234245A (en) * | 2011-05-06 | 2011-11-09 | 南京泽朗医药科技有限公司 | Method for preparing sulforaphane |
| US20130323225A1 (en) * | 2012-06-05 | 2013-12-05 | Jarrow Formulas, Inc. | Broccoli Based Nutritional Supplements |
| CN102949430A (en) * | 2012-11-01 | 2013-03-06 | 上海中海龙高新技术研究院 | Maca capsule and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023036250A1 (en) * | 2021-09-08 | 2023-03-16 | 北京化工大学 | Drug used for treating prostatitis or prostatic hyperplasia |
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