CN106520858A - Extraction method for water-soluble dietary fibre of ginkgo leaf - Google Patents

Extraction method for water-soluble dietary fibre of ginkgo leaf Download PDF

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Publication number
CN106520858A
CN106520858A CN201610915862.6A CN201610915862A CN106520858A CN 106520858 A CN106520858 A CN 106520858A CN 201610915862 A CN201610915862 A CN 201610915862A CN 106520858 A CN106520858 A CN 106520858A
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soluble dietary
folium ginkgo
dietary fiber
water soluble
water
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CN106520858B (en
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苗敬芝
董玉玮
陈尚龙
李强
刘传申
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Shanghai Di Wan Electronic Technology Co.,Ltd.
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Xuzhou University of Technology
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/04Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds

Abstract

The invention belongs to the technical field of natural product extraction, and specifically relates to an extraction method for water-soluble dietary fibre of ginkgo leaf. According to the extraction method for the water-soluble dietary fibre of the ginkgo leaf, which is disclosed by the invention, enzymolysis is carried out through using cellulose and pectinase as a complex enzyme preparation, taking the ginkgo leaf as a raw material and taking water as an extraction agent, so as to extract the water-soluble dietary fibre, and the method is simple and convenient to operate, low in price and non-toxic; and moreover, the extracted water-soluble dietary fibre can be added into dairy products, beverages and other foods as a new natural green food additive, the healthcare function of the products is added, and a wide market prospect is provided for the comprehensive development and utilization of the ginkgo leaf. The transfer rate of the extraction of the method disclosed by the invention for the water-soluble dietary fibre is greater than 90%; and in the obtained extracted product, the purity of the water-soluble dietary fibre is greater than 85%, and high extraction reproducibility is achieved.

Description

A kind of extracting method of Folium Ginkgo water soluble dietary fiber
Technical field
The invention belongs to technical field of natural product extraction, and in particular to a kind of extraction of Folium Ginkgo water soluble dietary fiber Method.
Background technology
Ginkgo gymnosperm Ginkgoaceae Ginkgo deciduous tree plant, is subtropical zones, temperate zone seeds, extensively plants in China Training, is one of main economic tree of China.Research find ginkgo agent have to prevent and treat cardiovascular and cerebrovascular disease, senile dementia and Effect to anti-platelet activating factor, developed at present Gingko biloba plant medicine preparation, functional food, health product and All multi-products such as cosmetics, show obvious economic advantages.Current ginkgo agent product is more with gingko as active matter Matter, and the utilization at other positions is then less.
In fact there are some researches show, Folium Ginkgo also have very high medical value, such as promoting blood circulation and stopping pain, relieving diarrhea with astringents, hold back Lung is relievingd asthma.Ginkgo leaf nutrition enriches, and mainly has flavonoid, terpenoid, phenols, alkaloid etc., and contains more aqueous soluble dietary Fiber, is a kind of integration of edible and medicinal herbs material.Dietary fiber is divided into water soluble dietary fiber (SDF) and water-insoluble according to its dissolubility Dietary fiber (DF).Wherein SDF is more than DF to human body physiological function, and SDF has extensive nutritional health function, can prevent fertilizer The diseases such as fat disease, heart disease, diabetes, SDF can thoroughly be decomposed by the microorganism in intestinal, produce various short-chain fatty acid, Prevention and treatment to rectum cancer and colon cancer has certain effect, and SDF is conducive to the growth and breeding of the probioticss such as bacillus bifiduss, Gastrointestinal function can be improved.With the improvement of people's living standards, the emergence of all kinds of " ciril diseases " so that the weight of dietary fiber The property wanted gradually is recognized by people, how safely and efficiently to be prepared water soluble dietary fiber product, is increasingly learned both at home and abroad The attention of person.Therefore, the how further nutritive value of effective exploitation Folium Ginkgo, develops more gingko leaf preparation products, can Further expand the economic worth of Semen Ginkgo industry.
The content of the invention
For this purpose, the technical problem to be solved is to provide a kind of extraction side of Folium Ginkgo water soluble dietary fiber Method, to solve the problems, such as that Ginkgo Biloba Extract exploitation is poor in prior art.
For solving above-mentioned technical problem, the extracting method of Folium Ginkgo water soluble dietary fiber of the present invention, including such as Lower step:
(1) take dry Folium Ginkgo to crush, sieve, additions water is extractant, and add answering for cellulase and pectase Synthase agent carries out Enzymatic Extraction, obtains extracting solution;
(2) gained extracting solution is filtered, takes filtrate Jing and be concentrated under reduced pressure to give concentrated solution, take concentrated solution precipitate with ethanol and be precipitated Thing, that is, obtain the Folium Ginkgo water soluble dietary fiber.
In step (1), the Enzymatic Extraction step is regulation pH value 4.5-5.5, -55 DEG C of controlled enzymatic hydrolysis temperature 45 C Digested.
In step (1), the addition of the cellulase is the 0.6-1.0wt% of the Folium Ginkgo raw materials quality, And preferably 0.8wt%;The addition of the pectase is the 0.5-0.8wt% of suffered Folium Ginkgo raw materials quality, and preferably 0.6wt%.
In step (1), the volume of the extractant water is 15ml/g- with the mass ratio of the Semen Ginkgo leaf raw material 30ml/g, and preferably 20ml/g.
In step (1), it is described regulation pH value the step of be using salicylic acid adjust.
In step (2), the step of the extracting solution is filtered be using by extracting solution in vacuum 0.08MPa- Under the conditions of 15 DEG C -30 DEG C of 0.10MPa and temperature, filtered using Medium speed filter paper, obtain filtrate.
In step (2), described concentrating under reduced pressure step is referred to gained filtrate in vacuum 0.08MPa-0.10MPa The 1/3 of initial filtrate volume is concentrated into under the conditions of -60 DEG C of temperature 50 C, concentrated solution is obtained.
In step (2), the precipitate with ethanol step is to add the ethanol of the 90-95wt% of 3-5 times of volume to carry out concentrated solution Precipitate with ethanol 36h-48h.
In step (2), also include the step of gained sediment is carried out into lyophilization, the cryodesiccated condition It is, less than 20Pa, to be dried totally under the conditions of -50 DEG C~-60 DEG C of condenser temperature in vacuum.
The invention also discloses being extracted the Folium Ginkgo water soluble dietary fiber for obtaining by methods described.
The extracting method of Folium Ginkgo water soluble dietary fiber of the present invention adopts cellulase and pectase for compound enzyme Preparation, carries out enzymolysis and extraction water soluble dietary fiber with Folium Ginkgo as raw material, by extractant of water, not only easy to operate, cheap, It is nontoxic, and the water soluble dietary fiber for extracting can be added to the food such as milk product, beverage as new natural green food additive In product, the health care of product was both increased, also the comprehensive development and utilization for Folium Ginkgo provides wide market prospect.The present invention Methods described is extracted the rate of transform of water soluble dietary fiber and is more than 90%, and gained is extracted in product, water soluble dietary fiber purity More than 85%, and it is preferable to extract repeatability.
The health properties of Folium Ginkgo water soluble dietary fiber (SDF) of the present invention that accompanying drawing 1-4 shows and VC are contrasted, this Invention methods described extracts the Folium Ginkgo water soluble dietary fiber for obtaining, and can effectively remove OH, O2 -Free radical and to DPPH And NO2 -With preferable elimination efficiency, the health care of Folium Ginkgo water soluble dietary fiber (SDF) obtained in the method for the invention is imitated Fruit is better than the effect of VC.
Description of the drawings
In order that present disclosure is more likely to be clearly understood, the specific embodiment below according to the present invention is simultaneously combined Accompanying drawing, the present invention is further detailed explanation, wherein,
Fig. 1 is that Folium Ginkgo water soluble dietary fiber (SDF) of the present invention and VC are contrasted to the elimination effect of OH;
Fig. 2 is Folium Ginkgo water soluble dietary fiber (SDF) of the present invention and VC to O2 -The elimination effect contrast of free radical;
Fig. 3 is that Folium Ginkgo water soluble dietary fiber (SDF) of the present invention and VC are contrasted to the elimination effect of DPPH;
Fig. 4 is Folium Ginkgo water soluble dietary fiber (SDF) of the present invention and VC to NO2 -Elimination effect contrast.
Specific embodiment
In the following embodiments of the present invention, the detection of water soluble dietary fiber adopts phend-sulphuric acid, specifically includes:
1st, draw standard curve:Accurately pipette 0.00 with pipet, 0.10,0.20,0.40,0.60,0.80,1.00, In tool plug test tube, deionized water is supplemented to 2.00mL, plus 1.00mL to the glucose standards solution of 1.20mL (100 μ g/mL) 6% phenol solution, then rapid Deca 5.00mL concentrated sulphuric acid, shakes up, is cooled to room temperature, survey its absorbance under 490nm wavelength, With absorbance (Y) as vertical coordinate, map by abscissa of concentration of glucose (X), obtain equation of linear regression y=0.0564x+ 0.0167;R2=0.9987;
2nd, sample detection:Water soluble dietary fiber sample 0.25g is accurately weighed, is dissolved with warm water, quantitatively proceed to 250mL appearances In measuring bottle, constant volume shakes up, and accurately pipettes above-mentioned solution 25.00mL in 250mL volumetric flasks with pipet, deionized water constant volume, Shake up.After accurately pipetting dilution, solution 1.00mL is filled in test tube in tool, plus ionized water is supplemented to 2.00mL, adds 1.00mL 6% Phenol solution, shakes up, and then pipettes rapidly 5.00mL concentrated sulphuric acids in tool plug test tube, shakes up, survey absorbance, according to recurrence side Journey, calculates water soluble dietary fiber product purity.
Embodiment 1
Described in the present embodiment, the extracting method of Folium Ginkgo water soluble dietary fiber, comprises the steps:
(1) Folium Ginkgo drying is crushed into 50 mesh sieves, took the Folium Ginkgo 1kg after crushing, and add 20L water mixed for extractant It is even, cellulase 8g and pectase 6g is subsequently added, solution ph is adjusted as 4.8 with salicylic acid after mixing, temperature 50 C is controlled, Complex enzyme hydrolysis 60min is carried out, extracting solution is obtained, the water soluble dietary fiber rate of transform is 95.10% in Jing inspection extracting solution;
(2) by extracting solution under the conditions of vacuum 0.08MPa, 25 DEG C of temperature, filtered using Medium speed filter paper, obtain filtrate;Will Filtrate is concentrated into the 1/3 of initial filtrate volume under the conditions of vacuum 0.09MPa, temperature 60 C, obtains concentrated solution;By concentrated solution plus The ethanol solution of 4 times of volumes 95wt% carries out precipitate with ethanol and processes 48h;After precipitate with ethanol, supernatant is removed, sediment fraction is placed in lyophilization Machine is less than 20Pa in vacuum, is dried totally, obtains Folium Ginkgo water soluble dietary fiber product under the conditions of -50 DEG C of condenser temperature.
After testing, the dietary fiber purity of the Folium Ginkgo water soluble dietary fiber product is 88.62%.
Embodiment 2
Described in the present embodiment, the extracting method of Folium Ginkgo water soluble dietary fiber, comprises the steps:
(1) Folium Ginkgo drying is crushed into 50 mesh sieves, took the Folium Ginkgo 1kg after crushing, and add 25L water mixed for extractant It is even, cellulase 9g and pectase 7g is subsequently added, solution ph is adjusted as 5.0 with salicylic acid after mixing, 48 DEG C of temperature is controlled, Complex enzyme hydrolysis 55min is carried out, extracting solution is obtained, the water soluble dietary fiber rate of transform is 94.56% in Jing inspection extracting solution;
(2) by extracting solution under the conditions of vacuum 0.09MPa, 25 DEG C of temperature, filtered using Medium speed filter paper, obtain filtrate;Will Filtrate is concentrated into the 1/3 of initial filtrate volume under the conditions of vacuum 0.08MPa, temperature 60 C, obtains concentrated solution;By concentrated solution plus The ethanol solution of 3 times of volumes 90wt% carries out precipitate with ethanol and processes 44h;After precipitate with ethanol, supernatant is removed, sediment fraction is placed in lyophilization Machine is less than 20Pa in vacuum, is dried totally, obtains Folium Ginkgo water soluble dietary fiber product under the conditions of -55 DEG C of condenser temperature.
After testing, the dietary fiber purity of the Folium Ginkgo water soluble dietary fiber product is 86.60%.
Embodiment 3
Described in the present embodiment, the extracting method of Folium Ginkgo water soluble dietary fiber, comprises the steps:
(1) Folium Ginkgo drying is crushed into 50 mesh sieves, took the Folium Ginkgo 1kg after crushing, and add 28L water mixed for extractant It is even, cellulase 7g and pectase 6.5g is subsequently added, solution ph is adjusted as 5.2 with salicylic acid after mixing, temperature 52 is controlled DEG C, complex enzyme hydrolysis 65min is carried out, extracting solution is obtained, in Jing inspection extracting solution, the water soluble dietary fiber rate of transform is 93.80%;
(2) by extracting solution under the conditions of vacuum 0.10MPa, 25 DEG C of temperature, filtered using Medium speed filter paper, obtain filtrate;Will Filtrate is concentrated into the 1/3 of initial filtrate volume under the conditions of vacuum 0.10MPa, temperature 50 C, obtains concentrated solution;By concentrated solution plus The ethanol solution of 5 times of volumes 95wt% carries out precipitate with ethanol and processes 40h;After precipitate with ethanol, supernatant is removed, sediment fraction is placed in lyophilization Machine is less than 20Pa in vacuum, is dried totally, obtains Folium Ginkgo water soluble dietary fiber product under the conditions of -60 DEG C of condenser temperature.
After testing, the dietary fiber purity of the Folium Ginkgo water soluble dietary fiber product is 87.26%.
Embodiment 4
Described in the present embodiment, the extracting method of Folium Ginkgo water soluble dietary fiber, comprises the steps:
(1) Folium Ginkgo drying is crushed into 50 mesh sieves, took the Folium Ginkgo 1kg after crushing, and add 15L water mixed for extractant It is even, cellulase 6g and pectase 8g is subsequently added, solution ph is adjusted as 4.5 with salicylic acid after mixing, 55 DEG C of temperature is controlled, Complex enzyme hydrolysis 60min is carried out, extracting solution is obtained, the water soluble dietary fiber rate of transform is 91.38% in Jing inspection extracting solution;
(2) by extracting solution under the conditions of vacuum 0.10MPa, 15 DEG C of temperature, filtered using Medium speed filter paper, obtain filtrate;Will Filtrate is concentrated into the 1/3 of initial filtrate volume under the conditions of vacuum 0.08MPa, temperature 50 C, obtains concentrated solution;By concentrated solution plus The ethanol solution of 4 times of volumes 95wt% carries out precipitate with ethanol and processes 36h;After precipitate with ethanol, supernatant is removed, sediment fraction is placed in lyophilization Machine is less than 20Pa in vacuum, is dried totally, obtains Folium Ginkgo water soluble dietary fiber product under the conditions of -55 DEG C of condenser temperature.
After testing, the dietary fiber purity of the Folium Ginkgo water soluble dietary fiber product is 83.59%.
Embodiment 5
Described in the present embodiment, the extracting method of Folium Ginkgo water soluble dietary fiber, comprises the steps:
(1) Folium Ginkgo drying is crushed into 50 mesh sieves, took the Folium Ginkgo 1kg after crushing, and add 30L water mixed for extractant It is even, cellulase 10g and pectase 5g is subsequently added, solution ph is adjusted as 5.5 with salicylic acid after mixing, temperature 45 is controlled DEG C, complex enzyme hydrolysis 60min is carried out, extracting solution is obtained, in Jing inspection extracting solution, the water soluble dietary fiber rate of transform is 91.43%;
(2) by extracting solution under the conditions of vacuum 0.08MPa, 30 DEG C of temperature, filtered using Medium speed filter paper, obtain filtrate;Will Filtrate is concentrated into the 1/3 of initial filtrate volume under the conditions of vacuum 0.10MPa, 55 DEG C of temperature, obtains concentrated solution;By concentrated solution plus The ethanol solution of 4 times of volumes 95wt% carries out precipitate with ethanol and processes 48h;After precipitate with ethanol, supernatant is removed, sediment fraction is placed in lyophilization Machine is less than 20Pa in vacuum, is dried totally, obtains Folium Ginkgo water soluble dietary fiber product under the conditions of -55 DEG C of condenser temperature.
After testing, the dietary fiber purity of the Folium Ginkgo water soluble dietary fiber product is 83.18%.
Comparative example 1
Described in this comparative example, the extracting method of Folium Ginkgo water soluble dietary fiber is same as Example 1, and which differs only in PH value is adjusted using HCl in step (1).
After testing, the dietary fiber purity of the Folium Ginkgo water soluble dietary fiber product is 58.27%.Obviously, it is above-mentioned Embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.It is common for art For technical staff, can also make other changes in different forms on the basis of the above description.Here need not All of embodiment cannot be exhaustive.And thus it is extended obvious change or change still in the present invention Among the protection domain of creation.

Claims (10)

1. a kind of extracting method of Folium Ginkgo water soluble dietary fiber, it is characterised in that comprise the steps:
(1) take dry Folium Ginkgo to crush, sieve, addition water is extractant, and adds the compound enzyme of cellulase and pectase Agent carries out Enzymatic Extraction, obtains extracting solution;
(2) gained extracting solution is filtered, takes filtrate Jing and be concentrated under reduced pressure to give concentrated solution, take concentrated solution precipitate with ethanol and be precipitated thing, i.e., Obtain the Folium Ginkgo water soluble dietary fiber.
2. the extracting method of Folium Ginkgo water soluble dietary fiber according to claim 1, it is characterised in that the step (1), in, for adjusting pH value 4.5-5.5, -55 DEG C of controlled enzymatic hydrolysis temperature 45 C is digested the Enzymatic Extraction step.
3. the extracting method of Folium Ginkgo water soluble dietary fiber according to claim 1 and 2, it is characterised in that the step Suddenly in (1), the addition of the cellulase is the 0.6-1.0wt% of the Folium Ginkgo raw materials quality, and the pectase adds Dosage is the 0.5-0.8wt% of suffered Folium Ginkgo raw materials quality.
4. the extracting method of the Folium Ginkgo water soluble dietary fiber according to any one of claim 1-3, it is characterised in that institute State in step (1), the volume of the extractant water is 15ml/g-30ml/g with the mass ratio of the Semen Ginkgo leaf raw material.
5. the extracting method of the Folium Ginkgo water soluble dietary fiber according to any one of claim 1-4, it is characterised in that institute State in step (1), it is described regulation pH value the step of be using salicylic acid adjust.
6. the extracting method of the Folium Ginkgo water soluble dietary fiber according to any one of claim 1-5, it is characterised in that institute State in step (2), the step of the extracting solution is filtered be using by extracting solution in vacuum 0.08MPa-0.10MPa and temperature 15 Under the conditions of DEG C -30 DEG C, filtered using Medium speed filter paper, obtain filtrate.
7. the extracting method of the Folium Ginkgo water soluble dietary fiber according to any one of claim 1-6, it is characterised in that institute State in step (2), described concentrating under reduced pressure step is referred to gained filtrate in vacuum 0.08MPa-0.10MPa and temperature 50 The 1/3 of initial filtrate volume is concentrated under the conditions of DEG C -60 DEG C, concentrated solution is obtained.
8. the extracting method of the Folium Ginkgo water soluble dietary fiber according to any one of claim 1-7, it is characterised in that institute State in step (2), the precipitate with ethanol step is to add the ethanol of the 90-95wt% of 3-5 times of volume to carry out precipitate with ethanol 36h- concentrated solution 48h。
9. the extracting method of the Folium Ginkgo water soluble dietary fiber according to any one of claim 1-8, it is characterised in that institute State in step (2), also include the step of gained sediment is carried out into lyophilization, the cryodesiccated condition is in vacuum Less than 20Pa, it is dried totally under the conditions of -50 DEG C~-60 DEG C of condenser temperature.
10. the Folium Ginkgo water soluble dietary fiber for obtaining is extracted by any one of claim 1-9 methods described.
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