CN105132501A - Preparation method of rape pollen peptide solid extract - Google Patents
Preparation method of rape pollen peptide solid extract Download PDFInfo
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- CN105132501A CN105132501A CN201510564621.7A CN201510564621A CN105132501A CN 105132501 A CN105132501 A CN 105132501A CN 201510564621 A CN201510564621 A CN 201510564621A CN 105132501 A CN105132501 A CN 105132501A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses a preparation method of a rape pollen peptide solid extract, wherein the preparation method comprises the following steps: (1) extracting and removing wax and lipid ingredients in rape pollen by virtue of a supercritical CO2 fluid; (2) adding the dewaxed and degreased rape pollen to pure water, grinding and breaking by virtue of a colloid mill so as to obtain a syrupy liquid; (3) heating the syrupy liquid which is processed by the colloid mill to 90-95 DEG C and preserving heat for 30min, and then cooling to 50-55 DEG C; (4) hydrolyzing with the addition of proteolytic enzyme, heating and inactivating enzyme after hydrolysis, and cooling to 4-10 DEG C; (5) centrifuging the liquid obtained from enzymatic hydrolysis respectively by virtue of a decanter centrifuge and a disc centrifuge; (6) collecting centrifuged supernatant liquid, decompressing and concentrating until solid content is 45-65% so as to obtain a concentrate extract; and (7) drying the concentrate extract by virtue of vacuum belt-type liquid continuous drying equipment so as to obtain a rape pollen peptide extract. The preparation method disclosed by the invention, by a way of combining supercritical CO2 fluid extraction and biological enzymatic hydrolysis, can be used for preparing the solid rape pollen peptide extract which is good in solubility and is more conducive to absorption.
Description
Technical field
The present invention relates to a kind of method utilizing Pollen Brassicae campestris to prepare Pollen Brassicae campestris peptide solid extract.
Background technology
Pollen is the golden yellow powdery particles in plant flower, and as the elite of plant, pollen almost contains all nutrients of natural complete nutrients matter and human body needs.At present, scientist has found the nearly 300 kinds of nutrition source materials of 13 large class from pollen, these nutritive ingredients all have various different health protection effect, and also also exist between them improve and the proportioning of equilibrium, guarantee pollen, to human body, not only there is completely balanced health protection effect, and have obviously effect of uniqueness to the disease of the most organ of human body.China's geographical environment vast in territory and diversified, providing and contain the pollen resource infinitely abundant, kind is ten hundreds of, is inexhaustible, inexpensive natural nutrition source.
Rape is the main oil crops of China's tradition, and plantation region is wide, and cultivated area is up to 7.2 × 106hm2.In addition, the rape florescence is long, and pollen yield is large, so Pollen Brassicae campestris is the most large bee pollen of China, in China's pollen, occupies very important status.Now there are some researches show, the carbohydrate, amino acid, lipid acid, micro-VITAMIN etc. of Pollen Brassicae campestris not only containing needed by human body is also containing abundant other biologically active substance such as flavonoid compound, enzyme.The health-care effect that these nutritive ingredients have it certain such as improves immunizing power, delays senility, plays restraining effect etc. to hyperplasia of prostate.Therefore Pollen Brassicae campestris has enjoyed people to pay close attention to as protective foods.
But the market of Pollen Brassicae campestris is also in the raw material preliminary working stage at present, after just being removed honeybee limbs, through simple packing, packaging, does not have intensive processing product.Because the roughing product of Pollen Brassicae campestris exist poorly soluble, have allergen, therefore also really do not come in the life of consumers in general.
Summary of the invention
Object of the present invention provides a kind of method utilizing Pollen Brassicae campestris to prepare Pollen Brassicae campestris peptide solid extract.The invention provides a kind of deep process technology of Pollen Brassicae campestris, by Pollen Brassicae campestris after series of process process, adopt biological enzyme digestion method, obtain the solid Pollen Brassicae campestris peptide extract that a kind of solubility is good, be more conducive to absorption.
The technical measures that the present invention takes are:
A preparation method for Pollen Brassicae campestris peptide solid extract, comprises the steps:
(1) supercritical CO is utilized
2fluid extraction removes wax in Pollen Brassicae campestris and lipid component;
(2) dewaxing, Pollen Brassicae campestris after degreasing are joined in pure water, utilize colloidal mill to grind broken paste liquid;
(3) paste liquid after milling treatment of colloid is heated to 90-95 DEG C of insulation 20-30min; (object one being heated to 90-95 DEG C is killing microorganisms; Two is the pollen protein appropriateness sex change making stripping; After be cooled to 50-55 DEG C)
(4) add proteolytic ferment, hydrolysis post-heating goes out enzyme, is cooled to 4-10 DEG C after the enzyme that goes out; (object being cooled to 4-10 DEG C is that material microorganism under the environment of low temperature is not easy breeding, is convenient to follow-up centrifugal)
(5) Horizontal helical type centrifuge and disc centrifuge is adopted to carry out centrifugal to the liquid after enzymolysis respectively;
(6) collect centrifugal after supernatant liquor, concentrating under reduced pressure, is concentrated into solid content between 45-65%, obtains concentrated solution medicinal extract;
(7) Pollen Brassicae campestris peptide extract is obtained after concentrated solution medicinal extract being utilized the drying of vacuum belt liquid continuous drying equipment.
In step (1), extraction temperature is 53-58 DEG C, and extractor pressure is 30-35Mpa, and extraction time is 1-1.5 hour.
In step (2), the mass ratio of Pollen Brassicae campestris and pure water is 1/7 ~ 1/12.
In step (4), proteolytic ferment be papoid, flavor protease, compound protease, bromeline one or more; Proteolysis enzyme-to-substrate mass ratio is 1-5 ‰.
In step (7), drying plant is vacuum belt liquid continuous drying equipment.
The invention has the beneficial effects as follows and utilize aforesaid method, can obtain the Pollen Brassicae campestris extract that the solubility of Pollen Brassicae campestris quality more than 40% is good, wherein small-molecular peptides (3-10 amino acid) content is between 15-20%.The most outstanding feature of the present invention is: (1) before to the process of Pollen Brassicae campestris biological enzymolysis, employs supercritical CO
2fluid extraction removes wax in Pollen Brassicae campestris and lipid component, this treatment process, significantly increases the stripping that follow-up Pollen Brassicae campestris is soaked into effective active matter in cell after in water, improves extract yield and (use supercritical CO
2the final extract yield of fluid extraction is the 40-45% of Pollen Brassicae campestris quality, does not use supercritical CO
2the final extract yield of fluid extraction is the 35-40% of Pollen Brassicae campestris quality.), add the clarity after extract dissolving simultaneously; (2) another feature of the present invention make use of protease hydrolysis technique, and carry out enzymolysis to the albumen of Pollen Brassicae campestris, obtain the small-molecular peptides in Pollen Brassicae campestris, small-molecular peptides content is between 15-20%; (3) present invention employs horizontal helical type centrifugal centrifugal with video disc, centrifugal clarification degree is high, significantly improves than adopting the production efficiency of suction filtration and press filtration; (4) the present invention also has a distinguishing feature, in extracting method, employ vacuum belt liquid continuous drying equipment exactly carry out extract drying, because Pollen Brassicae campestris extract fusing point is low, viscosity is high, spraying dry is utilized to be easy to cause wall sticking phenomenon, collect less than dried powder, cannot industrialization produce; Utilize lyophilize, drying cost is high, and the production cycle is long; Using vacuum belt liquid continuous drying equipment to carry out drying to Pollen Brassicae campestris peptide is the drying process method that in the present invention, has a distinguishing feature, and rate of drying is faster than lyophilize, and energy consumption is low, and production cost is low.This invention technological method, the nutrient substance yield extracted from Pollen Brassicae campestris is high, and small-molecular peptides content is high, solubility is good, have high health value, this invention technological method improves the intensive processing state of the art of Pollen Brassicae campestris greatly, wide market.
Embodiment
Embodiment 1:
A preparation method for Pollen Brassicae campestris peptide solid extract, (1) gets 25kg Pollen Brassicae campestris to it is characterized in that it comprises the steps:, utilizes supercritical CO
2fluid extraction, extraction temperature is at 55 DEG C, and extractor pressure is at 35Mpa, and extraction 1h, removes wax and fat;
(2) dewaxing, Pollen Brassicae campestris after degreasing are joined in 250L pure water, utilize colloidal mill to grind broken paste liquid;
(3) paste liquid after milling treatment of colloid is heated to 90 DEG C insulation 30min, after be cooled to 55 DEG C;
(4) add 100g papain hydrolysis, hydrolysis 4h post-heating to 95 DEG C goes out enzyme, is cooled to 4 DEG C after the enzyme that goes out;
(5) Horizontal helical type centrifuge (3000rpm) and disc centrifuge (6000rpm) is adopted to carry out centrifugal to enzymolysis solution respectively;
(6) collect centrifugal after supernatant liquor, concentrating under reduced pressure, is concentrated into 25L, obtains concentrated solution medicinal extract;
(7) Pollen Brassicae campestris peptide extract is obtained after concentrated solution medicinal extract being utilized the drying of vacuum belt liquid continuous drying equipment.
Embodiment 2:
A preparation method for Pollen Brassicae campestris peptide solid extract, (1) gets 25kg Pollen Brassicae campestris to it is characterized in that it comprises the steps:, utilizes supercritical CO
2fluid extraction, extraction temperature is at 55 DEG C, and extractor pressure is at 30Mpa, and extraction 1h, removes wax and fat;
(2) dewaxing, Pollen Brassicae campestris after degreasing are joined in 150L pure water, utilize colloidal mill to grind broken paste liquid;
(3) paste liquid after milling treatment of colloid is heated to 95 DEG C insulation 25min, after be cooled to 50 DEG C;
(4) add 100g bromelain hydrolyzate, hydrolysis 4h post-heating to 95 DEG C goes out enzyme, is cooled to 10 DEG C after the enzyme that goes out;
(5) Horizontal helical type centrifuge (3000rpm) and disc centrifuge (6000rpm) is adopted to carry out centrifugal to enzymolysis solution respectively;
(6) collect centrifugal after supernatant liquor, concentrating under reduced pressure, is concentrated into 30L, obtains concentrated solution medicinal extract;
(7) Pollen Brassicae campestris peptide extract is obtained after concentrated solution medicinal extract being utilized the drying of vacuum belt liquid continuous drying equipment.
Embodiment 3:
A preparation method for Pollen Brassicae campestris peptide solid extract, (1) gets 25kg Pollen Brassicae campestris to it is characterized in that it comprises the steps:, utilizes supercritical CO
2fluid extraction, extraction temperature is at 55 DEG C, and extractor pressure is at 30Mpa, and extraction 1h, removes wax and fat;
(2) dewaxing, Pollen Brassicae campestris after degreasing are joined in 200L pure water, utilize colloidal mill to grind broken paste liquid;
(3) paste liquid after milling treatment of colloid is heated to 92 DEG C insulation 30min, after be cooled to 55 DEG C;
(4) add 500g papoid, flavor protease, compound protease, bromelain hydrolyzate, hydrolysis 4h post-heating to 95 DEG C goes out enzyme, is cooled to 4 DEG C after the enzyme that goes out;
(5) Horizontal helical type centrifuge (3000rpm) and disc centrifuge (6000rpm) is adopted to carry out centrifugal to enzymolysis solution respectively;
(6) collect centrifugal after supernatant liquor, concentrating under reduced pressure, is concentrated into 25L, obtains concentrated solution medicinal extract;
(7) Pollen Brassicae campestris peptide extract is obtained after concentrated solution medicinal extract being utilized the drying of vacuum belt liquid continuous drying equipment.
Embodiment 4:
A preparation method for Pollen Brassicae campestris peptide solid extract, (1) gets 25kg Pollen Brassicae campestris to it is characterized in that it comprises the steps:, utilizes supercritical CO
2fluid extraction, extraction temperature is at 55 DEG C, and extractor pressure is at 30Mpa, and extraction 1h, removes wax and fat;
(2) dewaxing, Pollen Brassicae campestris after degreasing are joined in 180L pure water, utilize colloidal mill to grind broken paste liquid;
(3) paste liquid after milling treatment of colloid is heated to 95 DEG C insulation 30min, after be cooled to 50 DEG C;
(4) add 500g papoid, 200g flavor protease, 300g compound protease, 200g bromelain hydrolyzate, hydrolysis 4h post-heating to 95 DEG C goes out enzyme, is cooled to 8 DEG C after the enzyme that goes out;
(5) Horizontal helical type centrifuge (3000rpm) and disc centrifuge (6000rpm) is adopted to carry out centrifugal to enzymolysis solution respectively;
(6) collect centrifugal after supernatant liquor, concentrating under reduced pressure, is concentrated into 30L, obtains concentrated solution medicinal extract;
(7) Pollen Brassicae campestris peptide extract is obtained after concentrated solution medicinal extract being utilized the drying of vacuum belt liquid continuous drying equipment.
Embodiment 5:
A preparation method for Pollen Brassicae campestris peptide solid extract, (1) gets 25kg Pollen Brassicae campestris to it is characterized in that it comprises the steps:, utilizes supercritical CO
2fluid extraction, extraction temperature is at 55 DEG C, and extractor pressure is at 30Mpa, and extraction 1h, removes wax and fat;
(2) dewaxing, Pollen Brassicae campestris after degreasing are joined in 230L pure water, utilize colloidal mill to grind broken paste liquid;
(3) paste liquid after milling treatment of colloid is heated to 90 DEG C insulation 35min, after be cooled to 55 DEG C;
(4) add 500g bromelain hydrolyzate, hydrolysis 4h post-heating to 95 DEG C goes out enzyme, is cooled to 4 DEG C after the enzyme that goes out;
(5) Horizontal helical type centrifuge (3000rpm) and disc centrifuge (6000rpm) is adopted to carry out centrifugal to enzymolysis solution respectively;
(6) collect centrifugal after supernatant liquor, concentrating under reduced pressure, is concentrated into 30L, obtains concentrated solution medicinal extract;
(7) Pollen Brassicae campestris peptide extract is obtained after concentrated solution medicinal extract being utilized the drying of vacuum belt liquid continuous drying equipment.
Claims (5)
1. a preparation method for Pollen Brassicae campestris peptide solid extract, is characterized in that comprising the steps:
(1) supercritical CO is utilized
2fluid extraction removes wax in Pollen Brassicae campestris and lipid component;
(2) dewaxing, Pollen Brassicae campestris after degreasing are joined in pure water, utilize colloidal mill to grind broken paste liquid;
(3) paste liquid after milling treatment of colloid is heated to 90-95 DEG C insulation 30min, after be cooled to 50-55 DEG C;
(4) add proteolytic ferment, hydrolysis post-heating goes out enzyme, is cooled to 4-10 DEG C after the enzyme that goes out;
(5) Horizontal helical type centrifuge and disc centrifuge is adopted to carry out centrifugal to the liquid after enzymolysis respectively;
(6) collect centrifugal after supernatant liquor, concentrating under reduced pressure, is concentrated into solid content between 45-65%, obtains concentrated solution medicinal extract;
(7) Pollen Brassicae campestris peptide extract is obtained after concentrated solution medicinal extract being utilized the drying of vacuum belt liquid continuous drying equipment.
2. method according to claim 1, is characterized in that: in step (1), and extraction temperature is 50-55 DEG C, and extractor pressure is 30-35Mpa, and extraction time is 1-1.5 hour.
3. method according to claim 1, is characterized in that: in step (2), and the mass ratio of Pollen Brassicae campestris and pure water is 1/7-1/12.
4. method according to claim 1, is characterized in that: in step (4), proteolytic ferment be papoid, flavor protease, compound protease, bromeline one or more; Proteolysis enzyme-to-substrate mass ratio is 1-5 ‰.
5. method according to claim 1, it is characterized in that: in step (7), drying mode adopts the dry concentrated extract of vacuum belt liquid continuous drying equipment, but not other drying plant is as spray drying device, freeze drying equipment, vacuum dryer.
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Cited By (5)
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CN105524963A (en) * | 2016-01-28 | 2016-04-27 | 浙江省医学科学院 | Broccoli polypeptide extract as well as preparation method and application thereof |
CN106860851A (en) * | 2017-02-09 | 2017-06-20 | 赵德润 | It is a kind of to prevent and treat rape pollen active peptide of prostatic disorders and preparation method thereof |
CN106947797A (en) * | 2017-03-05 | 2017-07-14 | 赵德润 | A kind of rape pollen active peptide and preparation method thereof |
CN107674116A (en) * | 2016-08-02 | 2018-02-09 | 北大方正集团有限公司 | A kind of purification process of Pneumocandin B0 |
CN114052113A (en) * | 2021-11-01 | 2022-02-18 | 菏泽尧舜牡丹生物科技有限公司 | Preparation method of pollen tablet candy |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105524963A (en) * | 2016-01-28 | 2016-04-27 | 浙江省医学科学院 | Broccoli polypeptide extract as well as preparation method and application thereof |
CN105524963B (en) * | 2016-01-28 | 2019-02-05 | 浙江省医学科学院 | Broccoli polypeptide extract and its preparation method and application |
CN107674116A (en) * | 2016-08-02 | 2018-02-09 | 北大方正集团有限公司 | A kind of purification process of Pneumocandin B0 |
CN106860851A (en) * | 2017-02-09 | 2017-06-20 | 赵德润 | It is a kind of to prevent and treat rape pollen active peptide of prostatic disorders and preparation method thereof |
CN106947797A (en) * | 2017-03-05 | 2017-07-14 | 赵德润 | A kind of rape pollen active peptide and preparation method thereof |
CN114052113A (en) * | 2021-11-01 | 2022-02-18 | 菏泽尧舜牡丹生物科技有限公司 | Preparation method of pollen tablet candy |
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