CN103468747B - Method for preparing vaccinium bracteatum thunb leaf pigment through enzymic method - Google Patents
Method for preparing vaccinium bracteatum thunb leaf pigment through enzymic method Download PDFInfo
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- CN103468747B CN103468747B CN201310452212.9A CN201310452212A CN103468747B CN 103468747 B CN103468747 B CN 103468747B CN 201310452212 A CN201310452212 A CN 201310452212A CN 103468747 B CN103468747 B CN 103468747B
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Abstract
The invention relates to a method for preparing vaccinium bracteatum thunb leaf pigment through the enzymic method, and belongs to the technical field of basic solution extraction. The vaccinium bracteatum thunb leaf pigment is prepared through the processes of enzyme source preparing, precursor solution preparing, enzymatic reacting and drying. The oxidase of vaccinium bracteatum thunb leaves is broken in a kill-out mode, and therefore the occurrence that the pigment of the vaccinium bracteatum thunb leaves is produced too early, the pigment is heated and damaged in the process of subsequent extraction and the quality of the pigment of the vaccinium bracteatum thunb leaves is affected can be avoided. According to the enzymatic reaction, fresh vaccinium bracteatum thunb leaf powder is added, the enzyme in the vaccinium bracteatum thunb leaves is directly utilized for oxidation, the enzyme source does not need to be bought additionally, and cost input can be reduced. The method is easy to carry out and short in production cycle, all needed devices are general devices used in modern industry production, and the method can be popularized easily.
Description
Technical field
The present invention relates to a kind of method that enzyme process prepares vaccinium bracteatum thunb leaf pigment, be specially the myrtillin leave after completing for raw material, utilize the enzyme of the fresh leaf of Fructus Vaccinii Bracteati itself to be prepared the method for vaccinium bracteatum thunb leaf pigment by biological enzymatic reaction, belong to stoste extractive technique field.
Background technology
Fructus Vaccinii Bracteati has another name called south candle, is Ericaceae Vaccinium plant, is extensively distributed in East Asia Region, comprises drought, Korea, Japan, Vietnam, the not distribution of other area, therefore external almost blank to Fructus Vaccinii Bracteati research, and studies in China ground zero.Research shows, vaccinium bracteatum thunb leaf pigment is oxidation (enzymatic oxidn) product of polyphenolic compound.This pigment can generate black-and-blue tunicle in a heated condition with albumen (as rice protein, Chicken Albumin, gelatin etc.), and non-refractory, oxidizable, have very strong physiologically active (China of Wei state. the extraction of vaccinium bracteatum thunb leaf pigment and character research [D]. Zhengzhou: He'nan University of Technology's master thesis, 2007).
Existing vaccinium bracteatum thunb leaf pigment extractive technique is divided into cured leaf to extract and fresh leaf extracts.The patent " a kind of method extracting pigments from bracteatum leaves " (application number: 201110264827.X) of Nanjing Zelang Pharmaceutical Technology Inc.'s application, the myrtillin leave of drying is pulverized by this invention, add acetum to soak, then extract, filtrate is obtained by filter screen, filtrate high speed centrifugation is separated, obtain supernatant liquor, supernatant liquor adds ultrafiltration in film separating system, nanofiltration, obtain concentrated solution, use ethanolic soln wash-out after poly-phthalein amine post absorption, elutriant concentrates, and namely lyophilize obtains vaccinium bracteatum thunb leaf pigment.The patent " a kind of method of extraction of natural melanin from myrtillin leave " (patent No.: ZL200510104210.6) that University Of Agriculture and Forestry In Fujian declares, this invention adopts cellulase or pectase preparation in conjunction with solvent extraction vaccinium bracteatum thunb leaf pigment.The people such as He'nan University of Technology is perhaps of heap of stone in addition, Southern Yangtze University Wang Li, Nanjing Forestry University Hu Zhijie and Jiang Ping adopt ethanol as Extraction solvent, be studied, determine the optimum extraction process of pigment to the Extraction of Pigment of myrtillin leave.Above extracting mode does not all relate to oxidation step, the melanochrome extracted can only calculate vaccinium bracteatum thunb leaf pigment precursor, be not real pigment (China of Wei state, Shao Bin, Xu Xinde. about new approaches [J] prepared by oriental blueberry melanin. Food Additives Used in China, 2011, (4): 135-138).
The patent " the melanic manufacture method of a kind of water miscible plant " (application number: 201110097948.X) of Zhejiang Medicine Co's application, this invention is that raw material manufactures melanin precursor with myrtillin leave, then manufactures plant melanochrome through operations such as polyphenol oxidase catalyzed oxidation, macroporous resin purification and spraying dry.Without de-enzyming process when in this invention, myrtillin leave is dry, before causing extraction, existing part phenolic compound and self enzyme reaction generate vaccinium bracteatum thunb leaf pigment, and in extraction, concentration process, other impurity of oxidation generation, then increases the lifting capacity of purifying.This invention also needs to add external source polyphenoloxidase in addition, increases cost.
Without patent " a kind of method prepared by vaccinium bracteatum thunb leaf pigment high efficiency extraction " (application number: 201310070246.1) fresh myrtillin leave water is cleaned that Sillim and safe Agri Biotech Pty Ltd. apply for, mechanical disintegration, add water 40 DEG C ~ 60 DEG C ultrasonic---microwave assisted techniques extracts, to extracting solution frozen centrifugation, remove precipitation, get supernatant liquor, microfiltration of ceramic membrane purifying, concentrated supernatant, vaccinium bracteatum thunb leaf pigment is prepared in lyophilize.The ceramic membrane purified concentration, the Freeze Drying Technique that adopt in this invention, production cost is higher.And fresh leaf is pulverized, first directly utilize self oxydasis to generate vaccinium bracteatum thunb leaf pigment, but vaccinium bracteatum thunb leaf pigment is extremely thermo-labile, this characteristic makes again membrane concentration irreplaceable.The fresh leaf of Fructus Vaccinii Bracteati is unfavorable for storing in addition, and this technological feasibility is restricted.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of enzyme process to prepare the method for vaccinium bracteatum thunb leaf pigment.
According to technical scheme provided by the invention, a kind of enzyme process prepares the method for vaccinium bracteatum thunb leaf pigment, and step is as follows:
(1) enzyme source preparation: fresh for Fructus Vaccinii Bracteati leaf is pulverized, rub cut, micronizing, directly use or under-16 DEG C ~-25 DEG C conditions preservation for subsequent use;
(2) precursor solution preparation: select the fresh leaf of raw Fructus Vaccinii Bracteati then, complete, 40 ~ 90 DEG C of dryings; Get dry myrtillin leave and add water, weight is 6 ~ 10 times of myrtillin leave weight, soaks 0.5 ~ 8h; Extract 2 times, being evaporated to density is 1.01 ~ 1.08g/cm
3;
(3) enzymatic reaction: add enzyme source prepared by step (1) in the precursor solution that step (2) prepares, contained Fructus Vaccinii Bracteati cured leaf quality in described precursor solution: enzyme source quality ratio is 5 ~ 50:1, at 20 ~ 37 DEG C, aeration-agitation reaction 3 ~ 6h, obtains enzymolysis solution; Stir speed (S.S.) is 100 ~ 800rpm, and air flow is 70 ~ 500L/min;
(4) dry: enzymolysis solution step (3) obtained is with the centrifugation of 2000 ~ 10000rpm, and filter, spraying dry or lyophilize, obtain product vaccinium bracteatum thunb leaf pigment.
Described in step (2), the mode of completing of myrtillin leave comprises: fried green, steaming green grass or young crops, baking, bubble green grass or young crops or radiation complete.
Described in step (2), Extracting temperature is 60 ~ 100 DEG C, preferably 60 ~ 80 DEG C.
Described in step (2), the temperature of concentrating under reduced pressure is 60 ~ 90 DEG C, preferably 60 ~ 75 DEG C.
Beneficial effect of the present invention: the present invention first destroys the oxydase of myrtillin leave self by completing, and avoids vaccinium bracteatum thunb leaf pigment to produce prematurely, and make it in the subsequent extracted course of processing because the reason such as to be heated is destroyed, affect pigment quality; Enzymatic reaction adopts and adds fresh myrtillin leave powder, directly utilizes enzyme in myrtillin leave to be oxidized, and without the need to buying enzyme source in addition, can reduce cost and dropping into; This technological operation is easy, with short production cycle, and the equipment used is all the general-purpose equipment in existing suitability for industrialized production, is beneficial to popularization.
Accompanying drawing explanation
Fig. 1 is black rice photo prepared by embodiment 1-3.
Fig. 2 is black rice photo prepared by comparative example 1.
Fig. 3 is black rice photo prepared by comparative example 2.
Embodiment
Embodiment 1
Enzyme process prepares a method for vaccinium bracteatum thunb leaf pigment, and step is as follows:
(1) enzyme source preparation: fresh for Fructus Vaccinii Bracteati leaf 5kg is pulverized, rub cut, micronizing, directly use or under-16 DEG C ~-25 DEG C conditions preservation for subsequent use;
(2) precursor solution preparation: select the fresh leaf 100kg of raw Fructus Vaccinii Bracteati then, fried green, 70 DEG C of dryings; Get dry myrtillin leave and add water, weight is 8 times of myrtillin leave weight, soaks 5h; Extract 2 times at 80 DEG C of temperature, being evaporated to density is 1.01g/cm
3;
(3) enzymatic reaction: add enzyme source prepared by step (1) in the precursor solution that step (2) prepares, contained Fructus Vaccinii Bracteati cured leaf quality in described precursor solution: enzyme source quality is than being 20:1, and aeration-agitation reaction 6h, obtains enzymolysis solution at 20 DEG C; Stir speed (S.S.) is 500rpm, and air flow is 500L/min;
(4) dry: enzymolysis solution step (3) obtained is with the centrifugation of 2000rpm, and filter, spraying dry or lyophilize, obtain product vaccinium bracteatum thunb leaf pigment.Inlet temperature 170 DEG C, air outlet temperature 70 DEG C.Obtain vaccinium bracteatum thunb leaf pigment 20.5kg brown-red powder.
Embodiment 2
Enzyme process prepares a method for vaccinium bracteatum thunb leaf pigment, and step is as follows:
(1) enzyme source preparation: fresh for Fructus Vaccinii Bracteati leaf 20kg is pulverized, rub cut, micronizing, directly use or under-16 DEG C ~-25 DEG C conditions preservation for subsequent use;
(2) precursor solution preparation: select the fresh leaf 100kg of raw Fructus Vaccinii Bracteati then, steams blue or green, 90 DEG C of dryings; Get dry myrtillin leave and add water, weight is 10 times of myrtillin leave weight, soaks 8h; Extract 2 times at 65 DEG C of temperature, being evaporated to density is 1.05g/cm
3;
(3) enzymatic reaction: add enzyme source prepared by step (1) in the precursor solution that step (2) prepares, contained Fructus Vaccinii Bracteati cured leaf quality in described precursor solution: enzyme source quality is than being 5:1, and aeration-agitation reaction 8h, obtains enzymolysis solution at 37 DEG C; Stir speed (S.S.) is 200 rpm, and air flow is 400L/min;
(4) dry: enzymolysis solution step (3) obtained is with the centrifugation of 10000rpm, and filter, spraying dry or lyophilize, obtain product vaccinium bracteatum thunb leaf pigment.Inlet temperature 180 DEG C, air outlet temperature 80 DEG C.Obtain vaccinium bracteatum thunb leaf pigment 19.2kg brown-red powder.
Embodiment 3
Enzyme process prepares a method for vaccinium bracteatum thunb leaf pigment, and step is as follows:
(1) enzyme source preparation: fresh for Fructus Vaccinii Bracteati leaf 16g is pulverized, rub cut, micronizing, directly use or under-16 DEG C ~-25 DEG C conditions preservation for subsequent use;
(2) precursor solution preparation: select the fresh leaf 800g of raw Fructus Vaccinii Bracteati then, baking, 40 DEG C of dryings; Get dry myrtillin leave and add water, weight is 6 times of myrtillin leave weight, soaks 0.5h; Extract 2 times at 90 DEG C of temperature, being evaporated to density is 1.08g/cm
3;
(3) enzymatic reaction: add enzyme source prepared by step (1) in the precursor solution that step (2) prepares, contained Fructus Vaccinii Bracteati cured leaf quality in described precursor solution: enzyme source quality is than being 50:1, and aeration-agitation reaction 4h, obtains enzymolysis solution at 28 DEG C; Stir speed (S.S.) is 100r/min, and air flow is 70L/min;
(4) dry: enzymolysis solution step (3) obtained is with the centrifugation of 8000rpm, and filter, lyophilize, obtains product vaccinium bracteatum thunb leaf pigment.Obtain vaccinium bracteatum thunb leaf pigment 245g brown-red powder.
Comparative example 1
The myrtillin leave that completes does not prepare pigment and dye rice effect experimental by fresh leaf enzymolysis oxidation
Select the fresh leaf 800g of raw Fructus Vaccinii Bracteati then, fried green, 70 DEG C of dryings; Get dry myrtillin leave and add water, weight is 6 times of myrtillin leave weight, soaks 0.5h; Extract 2 times at 90 DEG C of temperature, being evaporated to density is 1.08g/cm
3.Lyophilize, obtains the vaccinium bracteatum thunb leaf pigment precursor of lark powder.
Equivalent embodiment 1-3 gained vaccinium bracteatum thunb leaf pigment is mixed, gets 0.7g, be placed in 200mL beaker, add 35ml water stirring and dissolving, then add 25g rice, water proof boiling 0.5h, check dye meter Xiao Guo.
Meanwhile, get comparative example 1 gained vaccinium bracteatum thunb leaf pigment precursor 0.7g, be placed in 100ml beaker, add 35mL water stirring and dissolving, then add 25g rice, water proof boiling 0.5h, check dye meter Xiao Guo, contrast with the result of vaccinium bracteatum thunb leaf pigment.
Experiment proves, do not become taupe brown by the myrtillin leave extract dye rice that completes of fresh leaf enzymolysis, and be combined into black-and-blue tunicle by the myrtillin leave extract of fresh leaf enzymolysis and rice protein, the rice surface boiled is black-and-blue, and enzymolysis oxidation is the requisite step of preparation vaccinium bracteatum thunb leaf pigment.
Comparative example 2 myrtillin leave does not complete and dry contaminates rice effectiveness comparison with the dry extraction pigment that completes
Select the fresh leaf 800g of raw Fructus Vaccinii Bracteati then, dry (not completing), get dry myrtillin leave and add water, weight is 6 times of myrtillin leave weight, soaks 0.5h; Extract 2 times at 90 DEG C of temperature, being evaporated to density is 1.08g/cm
3.
Get fresh myrtillin leave 16g pulverize, rub cut, micronizing, add in concentrated solution, 28 DEG C are stirred enzymolysis 4h, pass into air simultaneously.
Centrifuging is carried out to reaction solution, lyophilize, obtain myrtillin leave extract.
Equivalent embodiment 1-3 gained vaccinium bracteatum thunb leaf pigment is mixed, gets 0.7g, be placed in 200ml beaker, add 35ml water stirring and dissolving, then add 25g rice, water proof boiling 0.5h, check dye meter Xiao Guo.
Meanwhile, get comparative example 2 gained myrtillin leave extract 0.7g, be placed in 200ml beaker, add 35ml water stirring and dissolving, then add 25g rice, water proof boiling 0.5h, check dye meter Xiao Guo, contrast with the result of vaccinium bracteatum thunb leaf pigment.
Experiment proves, the black meal cured leaf do not completed through extracting, concentrated, enzymolysis, dry preparation vaccinium bracteatum thunb leaf pigment dye rice be greyish-green, the product pigment that myrtillin leave prepared for raw material that is obviously worse than mutually to complete contaminates meter Xiao Guo.Therefore completing is the remarkable measure improving vaccinium bracteatum thunb leaf pigment quality.
Claims (3)
1. enzyme process prepares a method for black meal chromophyll, it is characterized in that step is as follows:
(1) enzyme source preparation: fresh for Fructus Vaccinii Bracteati leaf is pulverized, rub cut, micronizing, directly use or under-16 DEG C ~-25 DEG C conditions preservation for subsequent use;
(2) precursor solution preparation: select the fresh leaf of raw Fructus Vaccinii Bracteati then, complete, 40 ~ 90 DEG C of dryings; Get dry black meal leaf and add water, weight is 6 ~ 10 times of black meal leaf weight, soaks 0.5 ~ 8h; Extract 2 times at 60 ~ 100 DEG C of temperature, being evaporated to density is 1.01 ~ 1.08g/cm
3;
(3) enzymatic reaction: the enzyme source that in the precursor solution that step (2) prepares prepared by step (1), contained Fructus Vaccinii Bracteati cured leaf quality in described precursor solution: enzyme source quality ratio is 5 ~ 50:1, at 20 ~ 37 DEG C, aeration-agitation reaction 3 ~ 6h, obtains enzymolysis solution; Stir speed (S.S.) is 20 ~ 100 r/min, and air flow is 70 ~ 500L/min;
(4) dry: enzymolysis solution step (3) obtained, with the centrifugation of 2000 ~ 10000rpm, filters, spraying dry or lyophilize, obtain product crow meal chromophyll;
Described in step (2), the mode of completing of black meal leaf comprises: fried green, steaming green grass or young crops, baking, bubble green grass or young crops or radiation complete.
2. as claim 1 enzyme process prepares the method for black meal chromophyll, it is characterized in that: described in step (2), Extracting temperature is 60 ~ 80 DEG C.
3. as claim 1 enzyme process prepares the method for black meal chromophyll, it is characterized in that: described in step (2), the temperature of concentrating under reduced pressure is 60 ~ 75 DEG C.
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| CN104643060A (en) * | 2015-01-01 | 2015-05-27 | 吴中区木渎吴珍土特产商行 | Method for preparing food by using asiatic bilberry leaf extracting solution |
| CN108354111B (en) * | 2018-01-08 | 2022-05-17 | 浙江大学 | Natural colorant based on Vaccinium bracteatum leaves, and preparation method and application thereof |
| CN113383892A (en) * | 2021-07-01 | 2021-09-14 | 苏州求是本草健康科技有限公司 | Preparation method and application of dried leaves of oriental blueberry |
| CN117024988A (en) * | 2023-07-24 | 2023-11-10 | 浙江旺林生物科技有限公司 | Method for extracting Vaccinium bracteatum leaf melanin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939979A (en) * | 2005-09-30 | 2007-04-04 | 福建农林大学 | Extraction of natural melanin from myrtillin leaves |
| CN102356794A (en) * | 2011-10-16 | 2012-02-22 | 重庆市秀山红星中药材开发有限公司 | Processing method of honeysuckle tea |
| CN102747105A (en) * | 2011-04-19 | 2012-10-24 | 浙江医药股份有限公司新昌制药厂 | Method for preparing water-soluble plant melanin |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939979A (en) * | 2005-09-30 | 2007-04-04 | 福建农林大学 | Extraction of natural melanin from myrtillin leaves |
| CN102747105A (en) * | 2011-04-19 | 2012-10-24 | 浙江医药股份有限公司新昌制药厂 | Method for preparing water-soluble plant melanin |
| CN102356794A (en) * | 2011-10-16 | 2012-02-22 | 重庆市秀山红星中药材开发有限公司 | Processing method of honeysuckle tea |
Non-Patent Citations (2)
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