CN106543130A - A kind of preparation method of anthocyanidin - Google Patents

A kind of preparation method of anthocyanidin Download PDF

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Publication number
CN106543130A
CN106543130A CN201610952982.3A CN201610952982A CN106543130A CN 106543130 A CN106543130 A CN 106543130A CN 201610952982 A CN201610952982 A CN 201610952982A CN 106543130 A CN106543130 A CN 106543130A
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anthocyanidin
processed
preparation
extraction
jing steps
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CN201610952982.3A
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路新
魏晓琴
梁小思
张磊
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Ningxia Tianrui Industry Group Modern Agriculture Co Ltd
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Ningxia Tianrui Industry Group Modern Agriculture Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/58Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
    • C07D311/60Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
    • C07D311/62Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

Present invention relates particularly to a kind of preparation method of anthocyanidin, comprises the following steps:Material collection, drying, crushing, anthocyanidin extraction, concentration, distillation, dry, ultramicro grinding.Propyl alcohol of the extract using 95wt%, concentration extraction machine of the concentration using TS NS series, micronizer of the ultramicro grinding using 701 models of HMB, whole technique synergy finally give the powder of high anthocyanidin content.The invention provides a kind of process is simple, short easy to operate, extraction time, low production cost, the preparation method of the extraction anthocyanidin of environmental protection.

Description

A kind of preparation method of anthocyanidin
Technical field
The invention belongs to the extractive technique field of plant function active component, and in particular to a kind of preparation side of anthocyanidin Method.
Background technology
Anthocyanidin is a kind of water miscible phytochrome, belongs to flavone compound, more in the form of glucosides, is plant The main color-generation material of petal and fruit.Anthocyanidin is widely present in plant as a kind of secondary metabolites in plant body In the epidermal cell of petal, the cell tissue liquid of fruit and cauline leaf, exist in the vacuole of plant cell, can be turned by chlorophyll Change, color can be changed with the soda acid of cell liquid.Cell liquid is then partially red in acidity, and cell liquid is then partially blue in alkalescence.Flower Blue or green element is plant secondary metabolism product, is physiologically playing the part of important role.The color of petal and fruit can attract animal to carry out Pollination and seed dispersal.Anthocyanidin is the nutritious supplementary pharmaceutical of pure natural anti-aging, and research proves mankind nowadays and finds most have The antioxidant of effect, its antioxygenic property are higher by 50 times than vitamin E, are higher by 20 times than vitamin C.It is to human body Biological effectiveness is 100%, just can be detected in blood within 20 minutes after taking.It can not only prevent doing sth. in advance for wrinkle of skin Generate, can also maintain the stream that is stable, strengthening fine vascular circulation, raising capilary and vein of normal cell linkages, blood vessel It is dynamic, and then reach the rapid healing of abnormal skin.Anthocyanidin is natural sunlight overcover, is prevented from ultraviolet damage skin Skin, skin belong to connective tissue, and collagen contained therein and rigid albumen play an important role to the total of skin.
In recent years, due to the solid demand of domestic and international market, the gradually expansion of China's broccoli cultivated area, due to the country Increasing for broccoli yield, is brought therewith, substantial amounts of leaf and stem after broccoli processing or harvesting, accounts for plant 50%-60%'s Blade all by as discarded object, causes the environmental problems such as air pollution and body eutrophication after corruption.Such as Taizhou of Zhejiang Upper disk is the township of Chinese broccoli, and, up to more than 10 ten thousand mu, annual discarded broccoli stem-leaf is left up to 350,000 tons for broccoli cultivated area The right side, one to the busy season, and be thick on the ground broccoli stem-leaf, and pile up like a mountain, stinks to high heaven, have a strong impact on the daily life of the common people after rotting Environment living, not only causes the pollution of environment, also result in the waste of ample resources.Also contain in Jing investigation broccoli blades There is anthocyanidin, so the method that anthocyanidin is extracted in research from broccoli blade has important practical significance.
103420970 A of Chinese patent CN disclose a kind of method for extracting anthocyanidin.The method includes:1) flower will be contained Blue or green plain raw material, split-phase salt, deionized water and hydrophilic organic solvent mix lucifuge and carry out aqueous two-phase extraction, mutually extract in collection Liquid;2) by step 1) obtained by upper phase extract concentration, obtain anthocyanidin crude extract;3) by step 2) obtained by anthocyanidin crude extract Cross macroporous resin column to be adsorbed, the macroreticular resin after adsorption saturation, is cleaned with water, removal of impurities is until water lotion is colourless, then is used Eluent is eluted, and collects eluent, is dried, is obtained the anthocyanidin.102715605 A of Chinese patent CN disclose one The preparation process of blueberry concentrated juice of kind high anthocyanidin content, the invention be respectively adopted pectase blueberry pulp is carried out digesting, Shitosan obtains the blueberry juice clarified, reduced pressure concentration technique for fining agent and produces blueberry inspissated juice, microwave disinfection to blueberry concentration Juice carries out sterilization.105859674 A of Chinese patent CN disclose a kind of extracting method of pitaya peel anthocyanidin, including as follows Step:(1) pitaya peel powder;(2) pitaya peel powder solution;(3) ultrasonic wave extraction;(4) add acetic acid;(5) cross post;(6) Separate anthocyanidin.Methods of these traditional extraction anthocyanidin exist many technical process, extraction time length, production into The big problem of this height, extraction operation difficulty.
The content of the invention
The present invention is in order to overcome the defect of prior art, there is provided a kind of process is simple, easy to operate, extraction time be short, The preparation method of low production cost, the extraction anthocyanidin of environmental protection, the raw material for extracting anthocyanidin is selected from broccoli blade, so as to solve Broccoli blade pollutes the problem of environment, has expanded the plant source for extracting anthocyanidin again.
To achieve these goals, the technical solution adopted in the present invention is:
(1) material collection:Pick it is fresh, without rot, the broccoli blade without brown stain.
(2) dry:After the raw material that step (1) is collected is rinsed well, being placed in hot air drier carries out drying and processing.
(3) crush:The broccoli blade that Jing steps (2) were processed is crushed to into 40 mesh with airslide disintegrating mill, blade is obtained Powder.
(4) anthocyanidin is extracted:According to solid-liquid ratio 1:10, the blade powder that 95wt% propyl alcohol and Jing steps (3) were processed Mix, extraction time is 40min-80min, and Extracting temperature is 50 DEG C -70 DEG C, obtains extract.
(5) concentrate:The extract that Jing steps (4) were processed is carried out into extraction concentration, extract with thickener is extracted Material temperature degree is 98 DEG C, and concentration material temperature is 40 DEG C -60 DEG C, obtains concentrate.
(6) distill:The concentrate that Jing steps (5) were processed is carried out into distillation process, vapo(u)rizing temperature is 97.4 DEG C, is steamed Evaporate thing.
(7) it is dried:The distillation that Jing steps (6) were processed is dried into process, is dried to the moisture of distillation and is down to Below 8wt%, obtains dried object.
(8) ultramicro grinding:The dried object that Jing steps (7) were processed is carried out into ultramicro grinding process, is obtained final product containing anthocyanidin Powder.
(9) finished product:The powder containing anthocyanidin that Jing steps (8) are processed is tested quality treatment, quality inspection is closed Quantitative package after lattice, gets product.
Further, the drying temperature of the step (2) is 50-80 DEG C.
Further, the drying time of the step (2) is 4-8h.
Further, the model TS-NS series of the extraction thickener of the step (5).
Further, the drying equipment of the step (7) is hot air drier.
Further, model HMB-701 of the micronizer of the step (8).
Further, the smashing fineness index of the step (8) is 100 mesh.
Beneficial effect
The present invention improves the extraction flower of a kind of process is simple, short easy to operate, extraction time, low production cost, environmental protection The preparation method of blue or green element.Through material collection, drying, crushing, extraction, concentration, distillation, drying, ultramicro grinding, finished product packing etc. A series of PROCESS FOR TREATMENT, the synergy of each technique finally give the powder containing anthocyanidin 30-32wt%.
Raw material selected by the present invention is broccoli blade, and its wide material sources is with low cost, while being conducive to alleviating western orchid Cause the environmental problems such as air pollution, body eutrophication after a large amount of broccoli blades corruption discarded after flower processing or harvesting, Resource is made to be fully utilized.
Drying and processing is carried out to broccoli blade so that the moisture of broccoli blade is controlled within 10wt%, is had Help follow-up anthocyanidin to extract, fully ensure that concentration of the extract when anthocyanidin is extracted will not be too low, improve anthocyanidin Recovery rate.Pulverization process is carried out to broccoli blade, the recovery rate of anthocyanidin can be further improved.Made from 95wt% propyl alcohol For extract, the propyl alcohol of high-quality percentage is more easy to extract anthocyanidin.The extraction time 40-80min of selection, Extracting temperature 50- 70 DEG C, by testing the extraction rate reached for obtaining anthocyanidin within this range to peak.
Concentration is carried out to extract, selected TS-NS series extractions thickener floor space is little, and peripheral hardware only needs water And electricity, it is advantageously implemented substantial amounts of industrialized production;Set adopts SUS304 materials, and selection is excellent, inner and outer welding polishing 300 mesh, it is ensured that the security of material;It is incubated using three layers, heat insulation effect is excellent, it is ensured that material is being the quilt at stable temperature Extract concentration;The design of open type, is easy to CIP cleaning devices are equipped with feeding intake and discharging for material, tank, is easy to equipment to clean, The process time is saved, continuous prodution is realized;Fuselage adopts cambered design, material without heating and to clean dead angle in tank, can Discharge completely, does not result in the wasting of resources;Using central controller controls, it is capable of achieving to extract the control and display of thickening temperature, High degree of automation, it is simple to operate;Concentrated using Dynamic Extraction, efficiency high.
Distillation process is carried out to concentrate, the propyl alcohol remained in concentrate can be evaporated, improve the pure of anthocyanidin Degree, while also ensure that the security of anthocyanidin.Process is dried to distillation, is in order to will be the moisture of distillation near Below 8wt%, improves the quality of anthocyanidin, while storage of being also more convenient for.
Carry out ultramicro grinding process to dried object, the special power of the micronizer fuselage of selected HMB-701 models Learn design so that the loss of machine consumptive material itself is few, and easy maintenance can be greatly lowered production cost;Can be continuous with 4 hours Work, can feed at any time and discharge at any time, can also adjust discharge fineness at any time, save the process time.Low cost is crushed, one is public Ultramicro grinding power consumption more than 1000 mesh of jin is less than 0.5 degree;Smashing fineness is high, is conducive to the extraction of anthocyanidin, improves product Quality;Crush temperature it is low, be not added with cooling system HMB series pulverizer in the case of continuously running, the powder temperature of production Can never be more than 45 degree, it is ensured that anthocyanidin will not scatter and disappear under high temperature activity again, while costliness can be saved and taken up an area Cooling facility, reduces production cost;String can be good at crushing while effective active composition therein will not be destroyed; Pollution-free to material, special force way ensures that not having big abrasion with material contact portion produces, it is possible to very well Guarantee material cleanliness factor.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate this It is bright rather than for limiting the scope of the present invention.Unless stated otherwise, in embodiment, techniques not described means can be used Mode known in those skilled in the art is realized.To those skilled in the art, without departing substantially from essence of the present invention and model On the premise of enclosing, various modifications that the material component in these embodiments, consumption are carried out, replacement, improvement, these shapes of equal value Formula similarly falls within the application appended claims limited range.Special instruction, the design parameter limited by the present invention There should be admissible error range.
Embodiment 1
A kind of preparation method of anthocyanidin, comprises the steps:
(1) material collection:Pick it is fresh, without rot, the broccoli blade without brown stain.
(2) dry:After the raw material that step (1) is collected is rinsed well, being placed in hot air drier carries out drying and processing, Drying temperature is 50 DEG C, and drying time is 4h.
(3) crush:The broccoli blade that Jing steps (2) were processed is crushed to into 40 mesh with airslide disintegrating mill, blade is obtained Powder.
(4) anthocyanidin is extracted:According to solid-liquid ratio 1:10, the blade powder that 95wt% propyl alcohol and Jing steps (3) were processed Mix, extraction time is 40min, and Extracting temperature is 50 DEG C, obtains extract.
(5) concentrate:The extract that Jing steps (4) were processed is carried out into extraction concentration with the extraction thickener of TS-NS series Process, it is 98 DEG C to extract temperature of charge, and concentration material temperature is 40 DEG C, obtains concentrate.
(6) distill:The concentrate that Jing steps (5) were processed is carried out into distillation process, 97.4 DEG C of vapo(u)rizing temperature is distilled Thing.
(7) it is dried:The distillation hot air drier that Jing steps (6) were processed is dried into process, is dried to distillation The moisture of thing is down to 8wt%, obtains dried object.
(8) ultramicro grinding:The dried object that Jing steps (7) were processed is surpassed with the micronizer of HMB-701 models Crushing of Ultrafine process, smashing fineness index is 100 mesh, obtains final product the powder containing anthocyanidin 30wt%.
(9) finished product:The powder containing anthocyanidin that Jing steps (8) are processed is tested quality treatment, quality inspection is closed Quantitative package after lattice, gets product.
Embodiment 2
A kind of preparation method of anthocyanidin, comprises the steps:
(1) material collection:Pick it is fresh, without rot, the broccoli blade without brown stain.
(2) dry:After the raw material that step (1) is collected is rinsed well, being placed in hot air drier carries out drying and processing, Drying temperature is 80 DEG C, and drying time is 8h.
(3) crush:The broccoli blade that Jing steps (2) were processed is crushed to into 40 mesh with airslide disintegrating mill, blade is obtained Powder.
(4) anthocyanidin is extracted:According to solid-liquid ratio 1:10, the blade powder that 95wt% propyl alcohol and Jing steps (3) were processed Mix, extraction time is 80min, and Extracting temperature is 70 DEG C, obtains extract.
(5) concentrate:The extract that Jing steps (4) were processed is carried out into extraction concentration with the extraction thickener of TS-NS series Process, it is 98 DEG C to extract temperature of charge, and concentration material temperature is 60 DEG C, obtains concentrate.
(6) distill:The concentrate that Jing steps (5) were processed is carried out into distillation process, vapo(u)rizing temperature is 97.4 DEG C, is steamed Evaporate thing.
(7) it is dried:The distillation hot air drier that Jing steps (6) were processed is dried into process, is dried to distillation The moisture of thing is down to 7wt%, obtains dried object.
(8) ultramicro grinding:The dried object that Jing steps (7) were processed is surpassed with the micronizer of HMB-701 models Crushing of Ultrafine process, smashing fineness index is 100 mesh, obtains final product the powder containing anthocyanidin 30wt%.
(9) finished product:The powder containing anthocyanidin that Jing steps (8) are processed is tested quality treatment, quality inspection is closed Quantitative package after lattice, gets product.
Embodiment 3
A kind of preparation method of anthocyanidin, comprises the steps:
(1) material collection:Pick it is fresh, without rot, the broccoli blade without brown stain.
(2) dry:After the raw material that step (1) is collected is rinsed well, being placed in hot air drier carries out drying and processing, Drying temperature is 65 DEG C, and drying time is 6h.
(3) crush:The broccoli blade that Jing steps (2) were processed is crushed to into 40 mesh with airslide disintegrating mill, blade is obtained Powder.
(4) anthocyanidin is extracted:According to solid-liquid ratio 1:10, the blade powder that 95wt% propyl alcohol and Jing steps (3) were processed Mix, extraction time is 60min, and Extracting temperature is 60 DEG C, obtains extract.
(5) concentrate:The extract that Jing steps (4) were processed is carried out into extraction concentration with the extraction thickener of TS-NS series Process, it is 98 DEG C to extract temperature of charge, and concentration material temperature is 50 DEG C, obtains concentrate.
(6) distill:The concentrate that Jing steps (5) were processed is carried out into distillation process, vapo(u)rizing temperature is 97.4 DEG C, is steamed Evaporate thing.
(7) it is dried:The distillation hot air drier that Jing steps (6) were processed is dried into process, is dried to distillation The moisture of thing is down to 6wt%, obtains dried object.
(8) ultramicro grinding:The dried object that Jing steps (7) were processed is surpassed with the micronizer of HMB-701 models Crushing of Ultrafine process, smashing fineness index is 100 mesh, obtains final product the powder containing anthocyanidin 32wt%.
(9) finished product:The powder containing anthocyanidin that Jing steps (8) are processed is tested quality treatment, quality inspection is closed Quantitative package after lattice, gets product.

Claims (7)

1. a kind of preparation method of anthocyanidin, comprises the steps:
(1) material collection:Pick it is fresh, without rot, the broccoli blade without brown stain;
(2) dry:After the raw material that step (1) is collected is rinsed well, being placed in hot air drier carries out drying and processing;
(3) crush:The broccoli blade that Jing steps (2) were processed is crushed to into 40 mesh with airslide disintegrating mill, blade powder is obtained;
(4) anthocyanidin is extracted:According to solid-liquid ratio 1:10, the blade powder that 95wt% propyl alcohol and Jing steps (3) were processed is mixed, Extraction time is 40min-80min, and Extracting temperature is 50 DEG C -70 DEG C, obtains extract;
(5) concentrate:The extract that Jing steps (4) were processed is carried out into extraction concentration, extract material temperature with thickener is extracted Spend for 98 DEG C, concentration material temperature is 40 DEG C -60 DEG C, obtains concentrate;
(6) distill:The concentrate that Jing steps (5) were processed is carried out into distillation process, vapo(u)rizing temperature is 97.4 DEG C, is distilled Thing;
(7) it is dried:The distillation that Jing steps (6) were processed is dried into process, is dried to the moisture of distillation and is down to 8wt% Hereinafter, obtain dried object;
(8) ultramicro grinding:The dried object that Jing steps (7) were processed is carried out into ultramicro grinding process, the powder containing anthocyanidin is obtained final product End;
(9) finished product:The powder containing anthocyanidin that Jing steps (8) are processed is tested quality treatment, after quality inspection is qualified Quantitative package, gets product.
2. a kind of preparation method of anthocyanidin according to claim 1, it is characterised in that the drying temperature of the step (2) Spend for 50-80 DEG C.
3. the preparation method of a kind of anthocyanidin according to claim 1, it is characterised in that during the drying of the step (2) Between be 4-8h.
4. the preparation method of a kind of anthocyanidin according to claim 1, it is characterised in that the extraction of the step (5) is dense The model TS-NS series of contracting machine.
5. the preparation method of a kind of anthocyanidin according to claim 1, it is characterised in that the drying of the step (7) sets Standby is hot air drier.
6. a kind of preparation method of anthocyanidin according to claim 1, it is characterised in that the Ultramicro-powder of the step (8) Model HMB-701 of broken machine.
7. the preparation method of a kind of anthocyanidin according to claim 1, it is characterised in that the crushing of the step (8) is thin Degree index is 100 mesh.
CN201610952982.3A 2016-11-03 2016-11-03 A kind of preparation method of anthocyanidin Pending CN106543130A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104356107A (en) * 2014-11-27 2015-02-18 秦富英 Method for extracting cyanidin from purple yam peel
CN105532849A (en) * 2016-01-13 2016-05-04 甘肃农业大学 Drying method for broccoli leaves

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104356107A (en) * 2014-11-27 2015-02-18 秦富英 Method for extracting cyanidin from purple yam peel
CN105532849A (en) * 2016-01-13 2016-05-04 甘肃农业大学 Drying method for broccoli leaves

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
李向果: "《西兰花叶中硫代葡萄糖普和原花青素的生物学效价评定》", 《甘肃农业大学硕士学位论文》 *
杨夫臣, 吴江, 程建徽, 徐凯, 陈俊伟: "《葡萄果皮花色素的提取及其理化性质》", 《果树学报》 *
汪茂田: "《天然有机化合物提取分离与结构鉴定》", 30 September 2004, 化学工业出版社 *

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Application publication date: 20170329