CN104222889A

CN104222889A - Wolfberry soluble dietary fiber and preparation method thereof

Info

Publication number: CN104222889A
Application number: CN201410458150.7A
Authority: CN
Inventors: 赵兵; 赵庆生; 王晓东
Original assignee: Institute of Process Engineering of CAS
Current assignee: Institute of Process Engineering of CAS
Priority date: 2014-09-10
Filing date: 2014-09-10
Publication date: 2014-12-24
Anticipated expiration: 2034-09-10
Also published as: CN104222889B

Abstract

The invention relates to a wolfberry soluble dietary fiber and a preparation method thereof. The soluble dietary fiber is separated from medlar residues; the medlar residues comprise residues produced by producing wolfberry juice, wolfberry fruit wine, wolfberry polysaccharide, wolfberry aqueous extracts, wolfberry alcohol extracts and the like. The preparation method comprises the following steps of treating the wolfberry residues by an acidic liquid, an alkaline liquid or enzymes, performing solid-liquid separation on a treating liquid, concentrating a clear liquid, depositing ethanol, and drying to obtain the wolfberry soluble dietary fiber. The technology is simple; the requirement for equipment is low; the color of a product is relatively good, and the product is relatively high in dissolvability, expanding capacity, water-holding capacity and oil-holding capacity; the wolfberry soluble dietary fiber is suitable for developing health food or being used as a food additive.

Description

A kind of matrimony vine soluble dietary fiber and preparation method thereof

Technical field

The present invention relates to Biochemical Engineering technical field, be specifically related to a kind of matrimony vine soluble dietary fiber and preparation method thereof, particularly relate to a kind of matrimony vine slag utilizing plant produced Lycium chinense wine, LBP-X, wolfberry juice etc. to produce and be separated soluble dietary fiber obtained and preparation method thereof.

Background technology

In recent years, along with developing rapidly of wolfberry industry, the matrimony vine cultivated area in the whole nation has reached more than 100 ten thousand mu, 100 many enterprises are had to get involved matrimony vine field of deep, the capital participated in reaches more than 80 hundred million yuan, annual produce about 1.5 ten thousand tons of matrimony vine slags, these matrimony vine slags can not be utilized effectively for a long time, cause the great wasting of resources and environmental pollution.

At present, the matrimony vine residue of matrimony vine field of deep generation comprises: the residue that the matrimony vine residue that the residue that the matrimony vine residue that the matrimony vine residue that production juice from Chinese wolfberry produces, production matrimony vine water extract produce, the matrimony vine residue of production matrimony vine alcohol extract generation, the matrimony vine residue producing LBP-X generation, the matrimony vine residue producing Chinese wolfberry fruit wine generation, separation matrimony vine seed produce, production fermentation Chinese wolfberry fruit wine produce, production matrimony vine functional components (as wolfberry pigment, matrimony vine flavones, folium lycii flavine, matrimony vine betaine, matrimony vine zeaxanthin etc.) produce.

Again such as, below relate to the patent of matrimony vine deep processing, all do not relate to residue treatment.Such as, CN103130698A discloses a kind of from matrimony vine, the method of zeaxanthin is extracted in Chinese wolfberry fruit dregs, CN103549572A discloses a kind of Wolfberry fruit juice beverage and production technology thereof, CN1416730A discloses a kind of production method of wolfberry fruit juice powder, CN1038205A discloses a kind of preparation method of juice from Chinese wolfberry, CN103012612A discloses a kind of extracting method of LBP-X, CN101133833A discloses a kind of matrimony vine active polyoses producing method, CN1263108A Lycium polysaccharide extraction and purification process, CN102703279A discloses a kind of production technology of the Chinese wolfberry fruit wine that bubbles, CN103045424A discloses a kind of brewing method of dry-type medlar fruit wine, CN103289858A discloses a kind of medlar fresh fruit full juice fermented wine and preparation method thereof, CN1465691A discloses a kind of production method of Lycium chinense wine, CN103130698A discloses a kind of from matrimony vine, the method of zeaxanthin is extracted in Chinese wolfberry fruit dregs, CN102659741A discloses the extraction preparation method of active component in a kind of lycium barbarum, CN103467615A discloses a kind of preparation method of lycium barbarum oligosaccharide, CN103006899A discloses a kind of extraction and purification process of fruit of Chinese wolfberry general flavone, detection method and application thereof.

Dietary fiber is first put forward by Hipsley nineteen fifty-three, and the cellulose of formation plant cell wall, hemicellulose and these 3 kinds of compositions of lignin are called dietary fiber by him.Dietary fiber (Dietary fiber, DF) these neologisms are that H.C.Trowell in 1972 introduces first, and are defined as " the polysaccharide carbohydrate be not absorbed by the body and lignin " with 1976.Nineteen ninety-five, Definition of dietary fibre is by the United Nations FAO and U.S. FDA: in all constituents of various edible animals and plants, and the material be hydrolyzed does not occur by the effect of the digestive ferment of people.2000, Definition of dietary fibre is by US corn chemist association (AACC): DF is plant edible part and similar carbohydrate, they can not be digested and assimilated for human small intestine, but in the inner all or part of fermentation of large intestine, polysaccharide, oligosaccharide, lignin and plant substrates can be comprised.Definition of dietary fibre is by Chinese Soclety of Nutrition: dietary fiber is the polysaccharide that can not be immediately used by the body, namely can not digest by digestive ferment in the intestines and stomach of the mankind, and the polysaccharide utilized that is not absorbed by the body.This kind of polysaccharide, mainly from the complex carbohydrate of plant cell wall, also can be referred to as SNSP, i.e. the polysaccharide of non-alpha-glucans.

Dietary fiber can be divided into water miscible and non-water-soluble two kinds by dissolubility, and total dietary fiber is both sums:

1. total dietary fiber (TDF): comprise all components, as SNSP, lignin, resistant starch (comprising Retrograded Starch and modified starch) and maillard reaction product etc.

2. soluble dietary fiber (SDF): refer to not by human body alimentary canal enzymic digestion, but dissolve in warm water or hot water and its aqueous solution again can by the reppd part dietary fiber of the ethanol of 4 times of volumes, it mainly refers to stored substance in plant cell and secretion, also comprises part microbial polysaccharide and synthesis class polysaccharide as pectin, guar gum, alginate, glucan and fungi polysaccharide.

3. insoluble dietary fiber (IDF): refer to not by human body alimentary canal enzymic digestion and the part dietary fiber be insoluble in hot water, in IDF, one class forms the cellulose of plant cell wall, hemicellulose, insoluble pectin and lignin, first 3 kinds is polysaccharide macromolecular condensate, and lignin is aromatic series hydrocarbon polymer; Another kind of is chitin contained in the shellfish such as shrimp, crab epidermis.According to source difference, dietary fiber can be divided into vegetalitas, animality, microorganism, algal polysaccharides class and synthesis class dietary fiber.Vegetalitas source as cellulose, hemicellulose, lignin, pectin, Arabic gum, more sore glue, galactomannans etc.Animality source as chitin, shitosan, collagen etc.Microbe-derived as xanthans etc.Algal polysaccharides class is as alginate, carragheen, agar etc.Synthesis class as carboxymethyl cellulose etc.Wherein plant is the main source of dietary fiber, is also the class that investigation and application is maximum.

Dietary fiber has positive effect to human health, is preventing human intestines and stomach's tract disease and is safeguarding prominent function in gastrointestinal health.Early stage epidemiological study display, dietary fiber can prevent colon cancer, to a certain extent can treatment of chronic diseases, thus has the good reputation of " enteron aisle street cleaner ".Research shows, the diet of dietary fiber content abundance, is all to have special effect in prevention or in treatment diabetes.Dietary fiber can also delay and reduce the absorption of the harmful substances such as human body heavy metal, has and reduces and prevent harmful chemical to the toxic action of human body.In addition, dietary fiber can improve the edible quality of food, processing characteristics and appearance characteristics, and the purposes in food is very extensive.At present, regarding dietary fiber effect report is as follows:

(1) prevent constipation: dietary fiber can retain enteron aisle moisture, promote enterocinesia, intestinal contents volume is increased, stool is softening, thus easily through enteron aisle, gut flora is balanced.Meanwhile, dietary fiber can stimulate intestinal mucosa in enteron aisle, promotes gastrointestinal peristalsis, reduces food time of staying in enteron aisle, accelerate drainage rate, reach effect of Constipation.

(2) antiobesity action.After dietary fiber enters enteron aisle, satiety can be increased, food-intake significantly reduces, this mainly has very strong water absorption and swelling performance due to dietary fiber, water suction after dietary fiber with and expand, volume and weight increase several times, the absorption of dietary fiber can also suppress the absorption of sugar, regulate digestion and absorption function, reduce the accumulation of fat, thus reach the object of fat-reducing.

(3) clinical symptoms of diabetes-alleviating people.The extended residence time of food in intestines, reduce the absorptivity of glucose, improve diabetic condition etc. mainly owing to there is pectin in dietary fiber, glue is gluey Polysaccharides, and water-retaining property is extremely strong.Therefore, to diabetes-alleviating, there is good effect as rich pectous foods such as potatos.

(4) blood fat is reduced.Dietary fiber is also conducive to reducing blood fat, prevents and improves coronary heart disease, hypertension.In dietary fiber, pectin can in conjunction with cholesterol, and lignin can be combined with cholic acid, makes it directly discharge from ight soil, prevention gall stone.

(5) protective effect on cancer risk.Investigation result shows, and dietary fiber can give protection against cancer by toxin expelling, and its effect is that other nutrients cannot be replaced.The absorption of the harmful substances such as heavy metal in enteron aisle can be undertaken delaying and reducing by taking in dietary fiber, and the absorption of dietary fiber simultaneously can make the toxic action of harmful chemical to human body drop to minimum.After taking in dietary fiber, the time of staying of ight soil in enteron aisle can shorten, and promotes intestines peristalsis, reduces the time of staying of carcinogen, thus the pathological change reducing cancer is dangerous.

The invention provides the method utilizing matrimony vine slag to produce matrimony vine dietary fiber, the matrimony vine slag that current factory can be produced utilizes once again, has both solved a factory processes matrimony vine slag difficult problem, has turned waste into wealth simultaneously, for China's dietary fiber industry increases new kind, source of supplying raw materials.

Summary of the invention

The object of the present invention is to provide a kind of matrimony vine soluble dietary fiber and preparation method thereof, especially one isolated soluble dietary fiber and preparation method thereof from matrimony vine residue.

For reaching this goal of the invention, the present invention by the following technical solutions:

First aspect, the invention provides a kind of matrimony vine soluble dietary fiber, and described soluble dietary fiber refers to isolated soluble dietary fiber from matrimony vine.

As optimal technical scheme, described soluble dietary fiber is isolated matrimony vine soluble dietary fiber from matrimony vine residue.

Preferably, described matrimony vine residue be produce matrimony vine residue that juice from Chinese wolfberry produces, produce matrimony vine residue that matrimony vine water extract produces, produce matrimony vine residue that matrimony vine alcohol extract produces, produce matrimony vine residue that LBP-X produces, produce matrimony vine residue that Chinese wolfberry fruit wine produces, produce matrimony vine residue that fermentation Chinese wolfberry fruit wine produces, produce residue that matrimony vine functional components produces in one or at least two or more mixture.

Preferably, described matrimony vine functional component is wolfberry pigment, matrimony vine flavones, folium lycii flavine, matrimony vine betaine, the one in matrimony vine zeaxanthin or at least two or more mixture.

As optimal technical scheme, matrimony vine soluble dietary fiber of the present invention, composition is the one or at least two or more of pectin, glucan, soluble cellulose or solubility hemicellulose.

Second aspect, present invention also offers a kind of method utilizing matrimony vine slag to prepare matrimony vine soluble dietary fiber, comprises the following steps:

(1) raw material: matrimony vine slag;

(2) acid extractants: the acid solution adding 5 ~ 35 times of weight in matrimony vine slag, the preferably acid solution of 10 ~ 20 times of weight, the more preferably acid solution of 15 times of weight; Soak, then extract, extraction time is 0.5 ~ 10h, preferably 2 ~ 6h, more preferably 2.5h; Separation of Solid and Liquid, collects supernatant;

(3) concentrated: supernatant to be concentrated, is concentrated into solid content 10% ~ 65%, preferably 30% ~ 55%, more preferably 40%;

(4) precipitate: by concentration be 50 ~ 100% ethanol above-mentioned concentrate is precipitated; Preferably 70 ~ 95% ethanol precipitate above-mentioned concentrate; More preferably the ethanol of 80% precipitates above-mentioned concentrate;

(5) dry: sediment adopts the ethanol of 75 ~ 100% to clean; Drying is carried out to the sediment after washing, dried material is pulverized or grinding, obtains solubility matrimony vine dietary fiber;

Wherein, the acid solution described in step (2) is any one or at least two or more mixture in hydrochloric acid, acetic acid, citric acid, malic acid, oxalic acid, sulfuric acid, nitric acid, lactic acid; Acid strength is 0.1% ~ 10%, preferably 0.5 ~ 2%, more preferably 0.7%.

As the further improvement of such scheme, alkalinity extraction can also be adopted to prepare soluble dietary fiber, and step is as follows:

(1) raw material: matrimony vine slag;

(2) alkali extracts: the alkali lye adding 5 ~ 35 times of weight in matrimony vine slag, the preferably alkali lye of 10 ~ 20 times of weight, the more preferably acid solution of 15 times of weight; Soak, then extract, extract 0.5 ~ 4h, preferably 1 ~ 3h, more preferably 2.5h; Separation of Solid and Liquid, collects supernatant;

Alkali lye described in step (2) is the one in NaOH or KOH; Concentration of lye is 0.5 ~ 10%, preferably 0.5 ~ 3%, more preferably 0.9%.

As the further improvement of such scheme, first can also then adopt alkalinity extraction soluble dietary fiber with acid extractants, step is as follows:

(1) raw material: matrimony vine slag;

(2) acid extractants: the acid solution adding 5 ~ 30 times of weight in matrimony vine slag, the preferably acid solution of 10 ~ 20 times of weight, the more preferably acid solution of 15 times of weight; Soak; Extract after immersion, extraction time is 0.5 ~ 4h, preferably 1 ~ 3h, more preferably 2.5h; Separation of Solid and Liquid, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the alkali lye adding 2 ~ 25 times of weight in residue obtained to step (2), the preferably alkali lye of 10 ~ 20 times of weight, the more preferably acid solution of 15 times of weight; Extract 0.5 ~ 4h, preferably 1 ~ 3h, more preferably 2.5h; Separation of Solid and Liquid, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 10% ~ 65%, preferably 30% ~ 55%, more preferably 40%;

(5) precipitate: by concentration be 50 ~ 100% ethanol above-mentioned concentrate is precipitated; Preferably 70 ~ 95% ethanol precipitate above-mentioned concentrate; More preferably the ethanol of 80% precipitates above-mentioned concentrate;

(6) dry: sediment adopts the ethanol of 75 ~ 100% to clean; Drying is carried out to the sediment after washing, dried material is pulverized or grinding, obtains solubility matrimony vine dietary fiber;

Wherein, the acid solution described in step (2) is any one or at least two or more mixture in hydrochloric acid, acetic acid, citric acid, malic acid, oxalic acid, sulfuric acid, nitric acid, lactic acid; Acid strength is 0.1% ~ 10%, preferably 0.5 ~ 2%, more preferably 0.7%;

Alkali lye described in step (3) is the one in NaOH or KOH; Concentration of lye is 0.5 ~ 10%, preferably 0.5 ~ 3%, more preferably 0.9%.

As the further improvement of such scheme, first can also carry out alkali extraction, then alkali be extracted residue and carry out acid extractants, step is as follows:

(1) raw material: matrimony vine slag;

(2) alkali extracts: the alkali lye adding 5 ~ 30 times of weight in matrimony vine slag, the preferably alkali lye of 10 ~ 20 times of weight, the more preferably alkali lye of 15 times of weight; Soak; Extract after immersion, extraction time is 0.5 ~ 4h, preferably 1 ~ 3h, more preferably 2.5h; Separation of Solid and Liquid, collect supernatant, residue is for subsequent use;

(3) acid extractants: the acid solution adding 2 ~ 25 times of weight in residue obtained to step (2), the preferably acid solution of 10 ~ 20 times of weight, the more preferably acid solution of 15 times of weight; Extract 0.5 ~ 4h, preferably 1 ~ 3h, more preferably 2.5h; Separation of Solid and Liquid, collects supernatant;

Wherein, the alkali lye described in step (2) is the one in NaOH or KOH; Concentration of lye is 0.5 ~ 15%, preferably 0.5 ~ 3%, more preferably 0.9%;

Acid solution described in step (3) is any one or at least two or more mixture in hydrochloric acid, acetic acid, citric acid, malic acid, oxalic acid, sulfuric acid, nitric acid, lactic acid; Acid strength is 0.1% ~ 10%, preferably 0.5 ~ 2%, more preferably 0.7%.

As the optimization of above-mentioned several types extracting mode, wherein:

Step (2) or the middle extracting mode of step (3) can adopt heating to extract or ultrasonic extraction;

Described heating is extracted, and Extracting temperature remains on 60 ~ 100 DEG C, preferably 80 ~ 90 DEG C, more preferably 85 DEG C; Extraction time 0.5 ~ 3h, preferably 1 ~ 2h, more preferably 1.5h.

Described ultrasonic extraction, extraction conditions is power 5W ~ 1000W/L, preferred 50W ~ 100W/L, preferred 80W/L; Extraction time 0.5 ~ 2h, preferably 1 ~ 2h, more preferably 1.5h.

As the further optimization of above-mentioned several types extracting mode, wherein:

Step is soaked in (2), it is characterized in that, the feed liquid after immersion is extracted after pulverizing again;

Described pulverizing adopts colloid mill to carry out ultramicro grinding or adopts liquid micronizer to pulverize;

Step (2) or the middle solid-liquid separation method of step (3) adopt a kind of mode in 3-foot solid-liquid separating machine, disc separator, sedimentation centrifuge to carry out.

As the further optimization of above-mentioned preparation method, wherein:

Before with alcohol settling, extract can also adopt acid or alkali to regulate pH value of solution to 6.5 ~ 7.5, and preferred pH7.0, then carries out alcohol settling.

As optimal technical scheme, the preparation method of matrimony vine soluble dietary fiber of the present invention, enzyme process can also be adopted to prepare, and step is as follows:

(1) enzymolysis: matrimony vine slag and water are mixed, pulverizes to obtain wolfberry fruit syrup; Adjust ph is 3.0 ~ 7.0, preferable ph 3.5 ~ 6.5, more preferably pH value 5; Enzyme-addedly carry out enzymolysis;

The mass ratio of described matrimony vine slag and water is 1:5 ~ 1:30, preferred 1:10 ~ 1:15, more preferably 1:12;

In described pulverising step, the granularity after pulverizing is 100 ~ 600 orders, preferably 200 ~ 400 orders, more preferably 300 orders;

In described enzymolysis step, enzymolysis enzyme is the complex enzyme of a kind of or at least two or more composition in cellulase, hemicellulase, AMS, carbohydrase, arabanase, protease;

Hydrolysis temperature is 20 ~ 60 DEG C, preferably 30 ~ 50 DEG C, more preferably 45 DEG C; Enzymolysis time is 0.5 ~ 24h; Preferably 2 ~ 10h, more preferably 3h;

(2) go out enzyme: enzymolysis liquid is carried out go out enzyme, Separation of Solid and Liquid, collects filtrate;

Describedly go out in enzyme step, enzyme-removal temperature is 50 ~ 95 DEG C, preferred 80-90 DEG C, more preferably 88 DEG C, and the enzyme time of going out is 2min;

In described solid-liquid separation step, centrifuge is adopted to be tripod pendulum type batch centrifugal or horizontal centrifuge; With in described tripod pendulum type batch centrifugal centrifugation step, the order number of filter cloth is 200 ~ 500 orders, preferably 300 orders;

(3) concentrated: filtrate to be concentrated, is concentrated into solid content 10% ~ 65%, preferably 30% ~ 55%, more preferably 40%;

As optimal technical scheme, the ethanol pellet of above-mentioned all scheme gained, except common heated-air drying, forced air drying etc. can also be dry in the following ways:

The drying mode of the dietary fiber of alcohol settling gained adopts spraying dry, fluidized bed drying or freeze drying to carry out drying;

Wherein, described employing spraying dry, EAT is 120 ~ 220 DEG C, preferably 150 ~ 190 DEG C, preferably 180 DEG C;

Described employing fluidized bed drying, baking temperature is 60 ~ 95 DEG C, preferably 70 ~ 80 DEG C, more preferably 75 DEG C.

Compared with prior art, the present invention has following beneficial effect:

Present invention process is easy, equipment requirement is simple, product color better, there is higher dissolubility, expansive force, retention ability, hold oily power, wherein, retention ability reaches as high as 5.78g/g, and holding oily power is 1.59-2.93g/g, and swelling power reaches more than 5.07mL/g, and there is excellent cholesterol adsorption capacity, cholate adsorption capacity and nitrous acid adsorption capacity, be applicable to exploitation health food or use as food additives.

Detailed description of the invention

Technical scheme of the present invention is further illustrated below by detailed description of the invention.

Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.

Embodiment 1

(1) raw material: produce the matrimony vine residue that matrimony vine alcohol extract produces;

(2) acid extractants: the 0.7% salt acid soak adding 5 times of weight in matrimony vine slag, then extract, extraction time is 10h; Separation of Solid and Liquid, collects supernatant;

(3) concentrated: supernatant to be concentrated, is concentrated into solid content 10%;

(4) precipitate: by concentration be 100% ethanol above-mentioned concentrate is precipitated;

(5) dry: sediment adopts the ethanol of 75% to clean; Drying is carried out to the sediment after washing, dried material is pulverized or grinding, obtains solubility matrimony vine dietary fiber.

Embodiment 2

(1) raw material: produce the matrimony vine residue that fermentation Chinese wolfberry fruit wine produces;

(2) acid extractants: 10% citric acid adding 35 times of weight in matrimony vine slag soaks, and then extract, extraction time is 0.5; Separation of Solid and Liquid, collects supernatant;

(3) concentrated: supernatant to be concentrated, is concentrated into solid content 65%;

(4) precipitate: by concentration be 50% ethanol above-mentioned concentrate is precipitated;

(5) dry: sediment adopts the ethanol of 100% to clean; Drying is carried out to the sediment after washing, dried material is pulverized or grinding, obtains solubility matrimony vine dietary fiber.

Embodiment 3

(1) raw material: the matrimony vine residue mixture of the matrimony vine residue that production LBP-X produces, the matrimony vine residue producing Chinese wolfberry fruit wine generation, the generation of production fermentation Chinese wolfberry fruit wine;

(2) acid extractants: add 0.1% hydrochloric acid of 10 times of weight, acetic acid, citric acid, malic acid, mixed acid immersion in matrimony vine slag, then extract, extraction time is 2; Separation of Solid and Liquid, collects supernatant;

(3) concentrated: supernatant to be concentrated, is concentrated into solid content 30%;

(4) precipitate: be that 70% ethanol precipitates above-mentioned concentrate by concentration;

(5) dry: sediment adopts the ethanol of 85% to clean; Drying is carried out to the sediment after washing, dried material is pulverized or grinding, obtains solubility matrimony vine dietary fiber.

Embodiment 4

(1) raw material: produce the matrimony vine residue that juice from Chinese wolfberry produces;

(2) acid extractants: 0.5% acetic acid adding 20 times of weight in matrimony vine slag soaks, and then extract, extraction time is 6h;

(3) concentrated: supernatant to be concentrated, is concentrated into solid content 55%;

(4) precipitate: be that 95% ethanol precipitates above-mentioned concentrate by concentration;

(5) dry: sediment adopts the ethanol of 90% to clean; Drying is carried out to the sediment after washing, dried material is pulverized or grinding, obtains solubility matrimony vine dietary fiber.

Embodiment 5

(1) raw material: produce the matrimony vine residue that LBP-X produces;

(2) acid extractants: add 2% citric acid of 15 times of weight, malic acid, the immersion of oxalic acid mixed acid in matrimony vine slag, then extract, extraction time is 2.5h; Separation of Solid and Liquid, collects supernatant;

(3) concentrated: supernatant to be concentrated, is concentrated into solid content 40%;

(4) precipitate: by concentration be 80% ethanol above-mentioned concentrate is precipitated;

(5) dry: sediment adopts the ethanol of 80% to clean; Drying is carried out to the sediment after washing, dried material is pulverized or grinding, obtains solubility matrimony vine dietary fiber;

Embodiment 6

(1) raw material: produce the residue that matrimony vine functional components produces;

Described matrimony vine functional component is wolfberry pigment, matrimony vine flavones, folium lycii flavine, matrimony vine betaine, matrimony vine zeaxanthin.

(2) acid extractants: the mixed acid of 0.5% hydrochloric acid and lactic acid that add 16 times of weight in matrimony vine slag soaks, and then extract, extraction time is 5h; Separation of Solid and Liquid, collects supernatant;

(3) concentrated: supernatant to be concentrated, is concentrated into solid content 35%;

(4) precipitate: by concentration be 70% ethanol above-mentioned concentrate is precipitated;

(5) dry: sediment adopts the ethanol of 75% to clean; Drying is carried out to the sediment after washing, dried material is pulverized or grinding, obtains solubility matrimony vine dietary fiber;

Embodiment 7

(1) raw material: produce the matrimony vine residue that matrimony vine water extract produces;

(2) acid extractants: 0.9% acetic acid adding 25 times of weight in matrimony vine slag soaks, and then extract, extraction time is 5.5h; Separation of Solid and Liquid, collects supernatant;

(3) concentrated: supernatant to be concentrated, is concentrated into solid content 50%;

Embodiment 8

(1) raw material: be separated the residue that matrimony vine seed produces.

(2) acid extractants: add 6% sulfuric acid of 25 times of weight, nitric acid, the immersion of lactic acid mixed acid in matrimony vine slag, then extract, extraction time is 6h; Separation of Solid and Liquid, collects supernatant;

Embodiment 9

(2) alkali extracts: the 15%NaOH solution adding 5 times of weight in matrimony vine slag soaks, and then extracts, and extracts 0.52.5h; Separation of Solid and Liquid, collects supernatant;

Embodiment 10

(1) raw material: produce the matrimony vine residue that matrimony vine water extract produces.

(2) alkali extracts: the 0.5%NaOH solution adding 35 times of weight in matrimony vine slag soaks, and then extracts, and extracts 4h; Separation of Solid and Liquid, collects supernatant;

(5) dry: sediment adopts the ethanol of 100% to clean; Drying is carried out to the sediment after washing, dried material is pulverized or grinding, obtains solubility matrimony vine dietary fiber;

Embodiment 11

(2) alkali extracts: the 3%KOH solution adding 10 times of weight in matrimony vine slag, soaks, then extracts, and extracts 1h; Separation of Solid and Liquid, collects supernatant;

Embodiment 12

(1) raw material: produce the matrimony vine residue that LBP-X produces;

(2) alkali extracts: the 0.9%NaOH adding 15 times of weight in matrimony vine slag soaks, and then extracts, and extracts 2.5h; Separation of Solid and Liquid, collects supernatant;

(5) dry: sediment adopts the ethanol of 80% to clean; Drying is carried out to the sediment after washing, dried material is pulverized or grinding, obtains solubility matrimony vine dietary fiber.

Embodiment 13

(1) raw material: produce the matrimony vine residue that Chinese wolfberry fruit wine produces, the matrimony vine residue mixture of producing fermentation Chinese wolfberry fruit wine generation;

(2) alkali extracts: 0.6%NaOH and the KOH mixed solution adding 25 times of weight in matrimony vine slag, soaks, then extracts, and extracts 3h, Separation of Solid and Liquid, collects supernatant;

(3) concentrated: supernatant to be concentrated, is concentrated into solid content 75%;

Embodiment 14

(1) raw material: produce the one in the residue of matrimony vine functional components generation or at least two or more mixture;

Described matrimony vine functional component is wolfberry pigment, matrimony vine flavones, folium lycii flavine, matrimony vine betaine, matrimony vine zeaxanthin;

(2) alkali extracts: the 1%NaOH solution adding 15 times of weight in matrimony vine slag, soaks, then extracts, and extracts 2h; Separation of Solid and Liquid, collects supernatant;

Embodiment 15

(2) acid extractants: 2% hydrochloric acid solution adding 5 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 120min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 2000W, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 0.5%NaOH solution adding 25 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 1000W, and extraction time 1h is centrifugal, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 10%;

(5) precipitate: by concentration be 100% ethanol to be precipitated to ethanol final concentration to above-mentioned concentrate be 80%; And adopt the ethanol purge 2 times of 100%;

(6) dry: carry out spraying dry after above-mentioned sediment is water-soluble, EAT 180 DEG C, pulverizes dried material, obtains solubility matrimony vine dietary fiber.

Embodiment 16

(2) acid extractants: 0.5% acetic acid solution adding 15 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 60 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 2%NaOH solution adding 20 times of weight in residue obtained to step (2), 95 DEG C of hot water extracting, extracts 0.5h, centrifugal, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 45%;

(5) precipitate: by concentration be 75% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 75%;

(6) dry: carry out spraying dry after above-mentioned sediment is water-soluble, EAT 120 DEG C, pulverizes dried material, obtains solubility matrimony vine dietary fiber.

Embodiment 17

(2) acid extractants: 0.5% citric acid solution adding 22 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 100 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 6%NaOH solution adding 12 times of weight in residue obtained to step (2), 95 DEG C of hot water extracting, extracts 0.5h, centrifugal, collects supernatant;

(5) precipitate: by concentration be 75% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 2 times of 75%;

(6) dry: carry out spraying dry after above-mentioned sediment is water-soluble, EAT 160 DEG C, pulverizes dried material, obtains solubility matrimony vine dietary fiber.

Embodiment 18

(1) raw material: produce the matrimony vine residue that LBP-X produces;

(2) acid extractants: 0.9% malic acid solution adding 25 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 60 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 2%KOH solution adding 15 times of weight in residue obtained to step (2), 95 DEG C of hot water extracting, extracts 0.5h, centrifugal, collects supernatant;

(5) precipitate: by concentration be 95% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 85%;

(6) dry: carry out spraying dry after above-mentioned sediment is water-soluble, EAT 150 DEG C, grinds dried material, obtains solubility matrimony vine dietary fiber.

Embodiment 19

(1) raw material: produce the matrimony vine residue that Chinese wolfberry fruit wine produces;

(2) acid extractants: 10% oxalic acid solution adding 20 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 60 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 1%NaOH solution adding 20 times of weight in residue obtained to step (2), 95 DEG C of hot water extracting, extracts 0.5h, centrifugal, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 35%;

(5) precipitate: by concentration be 95% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 95%;

(6) dry: freeze drying to be carried out to above-mentioned sediment, dried material is pulverized, obtain solubility matrimony vine dietary fiber.

Embodiment 20

(2) acid extractants: 1.5% sulfuric acid solution adding 20 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 60 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 2%KOH solution adding 20 times of weight in residue obtained to step (2), 95 DEG C of hot water extracting, extracts 0.5h, centrifugal, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 35;

(5) precipitate: by concentration be 95% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 75%;

(6) dry: carry out fluidized bed drying to above-mentioned sediment, baking temperature 70 DEG C, drying time, 150min, pulverized dried material, obtained solubility matrimony vine dietary fiber.

Embodiment 21

(1) raw material: produce the matrimony vine residue that LBP-X produces;

(2) acid extractants: 0.5% salpeter solution adding 16 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 100W, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 0.5%NaOH solution adding 25 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 80W/L 1000W, extraction time 2h, centrifugal, collects supernatant;

(5) precipitate: by concentration be 95% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 55%;

(6) dry: carry out fluidized bed drying to above-mentioned sediment, baking temperature 85 DEG C, drying time, 60min, pulverized dried material, obtained solubility matrimony vine dietary fiber.

Embodiment 22

(1) raw material: produce the matrimony vine residue that LBP-X produces;

(2) acid extractants: 0.7% lactate buffer solution adding 33 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 100W, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 0.5%KOH solution adding 35 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 1000W/L, and extraction time 0.5h is centrifugal, collects supernatant;

(5) precipitate: by concentration be 85% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 80%;

(6) dry: carry out fluidized bed drying to above-mentioned sediment, baking temperature 80 DEG C, drying time, 120min, pulverized dried material, obtained solubility matrimony vine dietary fiber.

Embodiment 23

(1) raw material: produce juice from Chinese wolfberry the matrimony vine residue produced and the mixture producing the matrimony vine residue that matrimony vine water extract produces;

(2) acid extractants: 0.2% hydrochloric acid solution adding 15 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 100W, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 3%NaOH solution adding 22 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 1000W/L, and extraction time 0.5h is centrifugal, collects supernatant;

Embodiment 24

(1) raw material: produce matrimony vine alcohol extract the matrimony vine residue produced and the mixture producing the matrimony vine residue that LBP-X produces;

(2) acid extractants: 0.6% hydrochloric acid solution adding 21 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 100W, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 3%NaOH solution adding 32 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 1000W/L, and extraction time 0.5h is centrifugal, collects supernatant;

(6) dry: carry out spraying dry after above-mentioned sediment is water-soluble, EAT 220 DEG C, grinds dried material, obtains solubility matrimony vine dietary fiber.

Embodiment 25

(2) acid extractants: 2.5% hydrochloric acid solution adding 28 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 100W, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 1%KOH solution adding 21 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 50W/L, and extraction time 2h is centrifugal, collects supernatant;

Embodiment 26

(1) raw material: the matrimony vine residue that production Chinese wolfberry fruit wine produces, the matrimony vine residue producing fermentation Chinese wolfberry fruit wine generation, the mixture produced in the residue of wolfberry pigment generation;

(2) acid extractants: 3.5% hydrochloric acid solution adding 24 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 100W, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 1%NaOH solution adding 15 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 50W/L, and extraction time 2h is centrifugal, collects supernatant;

(5) precipitate: by concentration be 85% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 55%;

(6) dry: 50 DEG C of vacuum drying to be carried out to above-mentioned sediment, dried material is pulverized, obtain solubility matrimony vine dietary fiber.

Embodiment 27

(2) acid extractants: 1.5% acetum adding 22 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 100W, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 7%NaOH solution adding 10 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 50W/L, and extraction time 2h is centrifugal, collects supernatant;

(5) precipitate: by concentration be 75% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 65%;

(6) dry: carry out fluidized bed drying to above-mentioned sediment, baking temperature 85 DEG C, drying time, 70min, pulverized dried material, obtained solubility matrimony vine dietary fiber.

Embodiment 28

(2) acid extractants: 0.8% sulfuric acid solution adding 10 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 250W/L, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 4%KOH solution adding 5 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 580W/L, and extraction time 1.5h is centrifugal, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 55%;

(5) precipitate: by concentration be 85% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 75%;

(6) dry: carry out fluidized bed drying to above-mentioned sediment, baking temperature 80 DEG C, drying time, 90min, pulverized dried material, obtained solubility matrimony vine dietary fiber.

Embodiment 29

(2) acid extractants: 0.2% acetic acid solution adding 20 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 60 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 2%KOH solution adding 32 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 250W/L, and extraction time 2.5h is centrifugal, collects supernatant;

Embodiment 30

(1) raw material: the residue being separated the generation of matrimony vine seed with FRUCTUS LYCII;

(2) acid extractants: 0.9% acetic acid solution adding 35 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 80 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 9%KOH solution adding 21 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 550W/L, and extraction time 0.5h is centrifugal, collects supernatant;

(5) precipitate: by concentration be 55% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 95%;

(6) dry: carry out spraying dry after above-mentioned sediment is water-soluble, EAT 170 DEG C, pulverizes dried material, obtains solubility matrimony vine dietary fiber.

Embodiment 31

(1) raw material: produce the matrimony vine residue that LBP-X produces;

(2) acid extractants: 0.9% acetic acid solution adding 15 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 70 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 1%KOH solution adding 25 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 350W/L, and extraction time 2.5h is centrifugal, collects supernatant;

(5) precipitate: by concentration be 65% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 85%;

(6) dry: carry out spraying dry after above-mentioned sediment is water-soluble, EAT 150 DEG C, pulverizes dried material, obtains solubility matrimony vine dietary fiber.

Embodiment 32

(2) acid extractants: 0.8% acetic acid solution adding 28 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 90 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 1%KOH solution adding 25 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 150W/L, and extraction time 1.5h is centrifugal, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 40%;

Embodiment 33

(2) acid extractants: 1.5% acetic acid solution adding 25 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 100 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 0.8%KOH solution adding 25 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 50W/L, and extraction time 1.5h is centrifugal, collects supernatant;

Embodiment 34

(1) raw material: produce wolfberry pigment, matrimony vine flavones, folium lycii flavine, matrimony vine betaine, the residue that matrimony vine zeaxanthin produces;

(2) acid extractants: 1.5% acetic acid solution adding 20 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 85 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 1.5%KOH solution adding 25 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 50W/L, and extraction time 0.5h is centrifugal, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 30%;

(5) precipitate: by concentration be 75% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 80%;

Embodiment 35

(2) acid extractants: 6.5% acetic acid solution adding 20 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 60 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 0.5%KOH solution adding 20 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 500W/L, and extraction time 0.5h is centrifugal, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 65%;

(5) precipitate: by concentration be 95% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 80%;

Embodiment 36

(2) acid extractants: 3.5% acetic acid solution adding 15 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Carry out 60 DEG C of hot water extracting after immersion, extraction time is 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 2.5%KOH solution adding 15 times of weight in residue obtained to step (2), ultrasonic extraction under normal temperature condition, and extraction conditions is power 1000W/L, and extraction time 0.5h is centrifugal, collects supernatant;

(5) precipitate: by concentration be 85% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 65%;

(6) dry: forced air drying to be carried out to above-mentioned sediment, dried material is pulverized, obtain solubility matrimony vine dietary fiber.

Embodiment 37

(1) raw material: the mixture of the matrimony vine residue that the matrimony vine residue that production matrimony vine water extract produces, the matrimony vine residue of production matrimony vine alcohol extract generation, the matrimony vine residue producing LBP-X generation, the matrimony vine residue producing Chinese wolfberry fruit wine generation, production fermentation Chinese wolfberry fruit wine produce;

(2) acid extractants: 4.5% hydrochloric acid solution adding 35 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 200W/L, extraction time 1h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 3.5%NaOH solution adding 15 times of weight in residue obtained to step (2), 95 DEG C of hot water extracting, extracts 0.5h, centrifugal, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 80%;

(5) precipitate: by concentration be 55% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 70%;

(6) dry: vacuum drying to be carried out to above-mentioned sediment, dried material is pulverized, obtain solubility matrimony vine dietary fiber.

Embodiment 38

(2) acid extractants: 2.5% hydrochloric acid solution adding 32 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 700W/L, extraction time 1h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 2.5%NaOH solution adding 15 times of weight in residue obtained to step (2), 95 DEG C of hot water extracting, extracts 0.5h, centrifugal, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 70%;

(5) precipitate: by concentration be 55% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 55%;

Embodiment 39

(2) acid extractants: 1.5% hydrochloric acid solution adding 22 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 800W/L, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 2%NaOH solution adding 24 times of weight in residue obtained to step (2), 95 DEG C of hot water extracting, extracts 0.5h, centrifugal, collects supernatant;

(5) precipitate: by concentration be 55% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 85%;

Embodiment 40

(1) raw material: matrimony vine residue is produce the matrimony vine residue that juice from Chinese wolfberry produces, the mixture producing the matrimony vine residue that LBP-X produces;

(2) acid extractants: 1.5% hydrochloric acid solution adding 18 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 600W/L, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) alkali extracts: the 1%NaOH solution adding 15 times of weight in residue obtained to step (2), 95 DEG C of hot water extracting, extracts 0.5h, centrifugal, collects supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 60%;

(6) dry: carry out spraying dry after above-mentioned sediment is water-soluble, EAT 165 DEG C, pulverizes dried material, obtains solubility matrimony vine dietary fiber.

Embodiment 41

(2) alkali extracts: the 0.8%NaOH solution adding 25 times of weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 300W/L, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) acid extractants: 0.9% hydrochloric acid solution adding 25 times of matrimony vine slag weight in residue obtained to step (2), 95 DEG C of hot water extracting, extract 0.5h, centrifugal, collect supernatant;

(5) precipitate: by concentration be 65% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 75%;

Embodiment 42

(1) raw material: produce the matrimony vine residue that wolfberry pigment produces;

(2) alkali extracts: the 1.5%NaOH solution adding 22 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 500W/L, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) acid extractants: the solution adding 15 times of weight 0.9% hydrochloric acid in residue obtained to step (2), 95 DEG C of hot water extracting, extract 0.5h, centrifugal, collect supernatant;

(5) precipitate: by concentration be 55% ethanol above-mentioned concentrate is precipitated; And adopt the ethanol purge 3 times of 75%;

(6) dry: carry out spraying dry after above-mentioned sediment is water-soluble, EAT 175 DEG C, pulverizes dried material, obtains solubility matrimony vine dietary fiber.

Embodiment 43

(1) raw material: the matrimony vine residue producing Chinese holly pigment and flavones generation;

(2) alkali extracts: the 0.3%NaOH solution adding 35 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; , the feed liquid after immersion is extracted after pulverizing again; Pulverize and adopt colloid mill to carry out ultramicro grinding; Being crushed to granularity is 50 μm; Ultrasonic extraction under normal temperature condition after pulverizing, extraction conditions is power 80W/L, extraction time 1h; Adopt 3-foot solid-liquid separating machine centrifugal, collect supernatant, residue is for subsequent use;

(3) acid extractants: the solution adding 20 times of weight 0.6% hydrochloric acid in residue obtained to step (2), 95 DEG C of hot water extracting, extract 0.5h, centrifugal, collect supernatant;

(4) concentrated: the supernatant of step (2) with (3) gained to be merged, concentrates, be concentrated into solid content 50%;

Embodiment 44

(1) raw material: the matrimony vine residue producing folium lycii flavine and betaine generation;

(2) alkali extracts: the solution adding 30 times of matrimony vine slag weight 0.9%NaOH in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 50W/L, extraction time 1.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) acid extractants: the solution adding 20 times of weight 0.7% hydrochloric acid in residue obtained to step (2), 95 DEG C of hot water extracting, extract 0.5h, centrifugal, collect supernatant;

Embodiment 45

(1) raw material: the matrimony vine residue simultaneously producing LBP-X, pigment, flavones generation;

(2) alkali extracts: the 0.5%NaOH solution adding 20 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 1000W/L, extraction time 0.5h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) acid extractants: 0.8% hydrochloric acid solution adding 20 times of weight in residue obtained to step (2), 95 DEG C of hot water extracting, extract 0.5h, centrifugal, collect supernatant;

(6) dry: carry out spraying dry after above-mentioned sediment is water-soluble, EAT 215 DEG C, pulverizes dried material, obtains solubility matrimony vine dietary fiber.

Embodiment 46

(1) raw material: the matrimony vine residue simultaneously producing LBP-X, zeaxanthin generation;

(2) alkali extracts: the 1.5%NaOH solution adding 10 times of matrimony vine slag weight in matrimony vine slag; Carry out immersion 10min; Ultrasonic extraction under normal temperature condition after immersion, extraction conditions is power 5W/L, extraction time 2h; Centrifugal, collect supernatant, residue is for subsequent use;

(3) acid extractants: 0.9% hydrochloric acid solution adding 20 times of weight in residue obtained to step (2), 95 DEG C of hot water extracting, extract 0.5h, centrifugal, collect supernatant;

Embodiment 47

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:5; Pulverize to obtain wolfberry fruit syrup to 100 order, adjust ph is 3.0; Add cellulase; Carry out enzymolysis; Hydrolysis temperature is 45 DEG C; Enzymolysis time is 3h; The enzyme work of cellulase used is 25 ~ 30IU/ml;

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 88 DEG C, and the enzyme time of going out is 1min; Adopt tripod pendulum type batch centrifugal Separation of Solid and Liquid, the order number of filter cloth is 200 orders, collects filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 25.

Embodiment 48

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:5; Pulverize to obtain wolfberry fruit syrup to 100 order, adjust ph is 7.0; Enzymolysis is carried out with hemicellulase; Hydrolysis temperature is 60 DEG C; Enzymolysis time is 0.5h; The enzyme of cellulase used is lived as 50IU/ml;

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 50 DEG C, and the enzyme time of going out is 2min; Separation of Solid and Liquid, collects filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 26.

Embodiment 49

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:15; Pulverize to obtain wolfberry fruit syrup to 400 order, adjust ph is 6.5; Add the complex enzyme of cellulase, hemicellulase, AMS, carbohydrase composition; Carry out enzymolysis; Hydrolysis temperature is 50 DEG C; Enzymolysis time is 2h; The enzyme of cellulase used is lived as 25IU/ml;

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 80 DEG C, and the enzyme time of going out is 5min; Separation of Solid and Liquid, collects filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 27.

Embodiment 50

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:10; Pulverize to obtain wolfberry fruit syrup to 200 order, adjust ph is 6.5; Add the complex enzyme of cellulase, arabanase, protease composition; Carry out enzymolysis; Hydrolysis temperature is 45 DEG C; Enzymolysis time is 10h; The enzyme of cellulase used is lived as 15IU/ml; The enzyme of protease used is lived as 0.5AU/g;

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 58 DEG C, and the enzyme time of going out is 4min; Adopt centrifuge Separation of Solid and Liquid, the order number of filter cloth is 300 orders;

Collect filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 28.

Embodiment 51

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:15; Pulverize to obtain wolfberry fruit syrup to 300 order, adjust ph is 3.5; With the complex enzyme of hemicellulase, AMS, carbohydrase, arabanase, protease composition; Carry out enzymolysis; Hydrolysis temperature is 20 DEG C, and enzymolysis time is 24h; The enzyme of cellulase used is lived as 35IU/ml; The enzyme of protease used is lived as 2.0AU/g

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 50 DEG C, and the enzyme time of going out is 6min; Adopt horizontal centrifuge Separation of Solid and Liquid, collect filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 29.

Embodiment 52

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:12; Pulverize to obtain wolfberry fruit syrup to 500 order, adjust ph is 5; Add cellulase, carry out enzymolysis; Hydrolysis temperature is 45 DEG C, and enzymolysis time is 3h; The enzyme of cellulase used is lived as 10IU/ml;

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 95 DEG C, and the enzyme time of going out is 1min; Separation of Solid and Liquid, collects filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 30.

Embodiment 53

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:12; Pulverize to obtain wolfberry fruit syrup to 300 order, adjust ph is 5; Add the complex enzyme of cellulase, hemicellulase, AMS composition; Carry out enzymolysis; Hydrolysis temperature is 45 DEG C; Enzymolysis time is 3h; The enzyme work of cellulase used is 15 ~ 25IU/ml;

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 88 DEG C, and the enzyme time of going out is 2min; Separation of Solid and Liquid, collects filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 31.

Embodiment 54

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:20; Pulverize to obtain wolfberry fruit syrup to 400 order, adjust ph is 6.5 complex enzymes adding cellulase, AMS, protease composition; Carry out enzymolysis; Hydrolysis temperature is 45 DEG C; Enzymolysis time is 2h;

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 95 DEG C, the enzyme time of going out is 2min, and Separation of Solid and Liquid, collects filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 32.

Embodiment 55

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:30; Pulverize to obtain wolfberry fruit syrup to 300 order, adjust ph is 7.0; With the complex enzyme of hemicellulase, AMS, protease composition; Carry out enzymolysis; Hydrolysis temperature is 50 DEG C; Enzymolysis time is 10h;

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 50 ~ 95 DEG C, preferred 80-90 DEG C, and more preferably 88 DEG C, the enzyme time of going out is 2min; Centrifuge is adopted to be tripod pendulum type batch centrifugal or horizontal centrifuge; Separation of Solid and Liquid, collects filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 33.

Embodiment 56

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:12; Pulverize to obtain wolfberry fruit syrup to 300 order, adjust ph is 7.0, adds the complex enzyme of cellulase, AMS, protease composition; Carry out enzymolysis; Hydrolysis temperature is 45 DEG C; Enzymolysis time is 3h; The enzyme of cellulase used is lived as 25IU/ml; The enzyme of protease used is lived as 3AU/g;

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 88 DEG C, and the enzyme time of going out is 1min; Separation of Solid and Liquid, collects filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 34.

Embodiment 57

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:30, pulverizes to obtain wolfberry fruit syrup to 600 order, and adjust ph is 6.5; Add the complex enzyme of cellulase, hemicellulase, AMS, carbohydrase, composition; Carry out enzymolysis; Hydrolysis temperature is 45 DEG C; Enzymolysis time is 3h; The enzyme of cellulase used is lived as 20IU/ml;

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 95 DEG C, and the enzyme time of going out is 2min; Adopt horizontal centrifuge; Separation of Solid and Liquid, collects filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 35.

Embodiment 58

(1) enzymolysis: matrimony vine slag and water are mixed, the mass ratio of matrimony vine slag and water is 1:20, pulverizes to obtain wolfberry fruit syrup to 350 order, and adjust ph is 5.5; Add the complex enzyme of cellulase, AMS composition; Carry out enzymolysis; Hydrolysis temperature is 35 DEG C; Enzymolysis time is 3h; The enzyme of cellulase used is lived as 20IU/ml;

(2) go out enzyme: the enzyme that carried out by enzymolysis liquid going out, temperature are 85 DEG C, and the enzyme time of going out is 2min; Adopt horizontal centrifuge; Separation of Solid and Liquid, collects filtrate;

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 35.

Embodiment 59

(3) concentrated (4) precipitation (5) are dry, and step is with embodiment 35.

The enzymolysis of note: embodiment 47-59 tests the residue that the matrimony vine slag that adopts adopts with the embodiment that respective embodiment (3-5) step is corresponding.

Project is measured by the physicochemical property of the sample of embodiment 1-59 gained, comprise retention ability (g/g), hold oily power (g/g), the adsorption capacity (mg/g) of swelling power (mL/g), cholesterol adsorption capacity (mg/g), cholate adsorption capacity (mg/g), nitrite, measurement result is as shown in table 1.

Table 1

By table 1 can draw following some:

(1) the matrimony vine soluble dietary fiber adopting acid extractants to obtain, its retention ability is at 3.01-5.22g/g, holding oily power is 1.80-2.50g/g, swelling power is 5.07-7.29mL/g, cholesterol adsorption capacity is 3.5-10.2mg/g, cholate adsorption capacity is 32.1-83.1mg/g, and the adsorption capacity of nitrous acid is 15.0-49.9mg/g;

(2) alkali is adopted to extract the matrimony vine soluble dietary fiber obtained, its retention ability is at 3.20-5.51g/g, holding oily power is 1.94-2.72g/g, swelling power is 5.19-7.56mL/g, cholesterol adsorption capacity is 3.2-12.5mg/g, cholate adsorption capacity is 34.3-73.3mg/g, and the adsorption capacity of nitrous acid is 17.0-32.3mg/g;

(3) after adopting first acid extractants, alkali extracts the matrimony vine soluble dietary fiber obtained, its retention ability is at 3.38-5.69g/g, holding oily power is 1.71-2.69g/g, swelling power is 5.82-7.01mL/g, cholesterol adsorption capacity is 3.9-11.3mg/g, cholate adsorption capacity is 32.8-85.7mg/g, and the adsorption capacity of nitrous acid is 19.3-63.8mg/g;

(4) the matrimony vine soluble dietary fiber that after adopting first alkali to extract, acid extractants obtains, its retention ability is at 3.45-5.78g/g, holding oily power is 1.59-2.93g/g, swelling power is 5.34-7.19mL/g, cholesterol adsorption capacity is 3.1-10.8mg/g, cholate adsorption capacity is 37.2-81.6mg/g, and the adsorption capacity of nitrous acid is 12.7-53.5mg/g;

(5) the matrimony vine soluble dietary fiber adopting enzyme-squash techniqued to obtain, its retention ability is at 3.68-5.72g/g, holding oily power is 1.70-2.81g/g, swelling power is 5.53-7.68mL/g, cholesterol adsorption capacity is 3.6-11.1mg/g, cholate adsorption capacity is 35.4-82.9mg/g, and the adsorption capacity of nitrous acid is 18.3-58.2mg/g.

Analysis is carried out known by the physicochemical property obtaining matrimony vine soluble dietary fiber prepared by embodiment 1-59, the matrimony vine soluble dietary fiber that the present invention utilizes matrimony vine slag to prepare has excellent physicochemical property, be suitable for developing health food or using as food additives, there is important using value.

The above; be only part detailed description of the invention of the present invention, but protection scope of the present invention is not limited thereto, any those skilled in the art are in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.

Claims

1. a matrimony vine soluble dietary fiber, is characterized in that, described soluble dietary fiber is isolated soluble dietary fiber from matrimony vine residue.

2. matrimony vine soluble dietary fiber as claimed in claim 1, it is characterized in that, described matrimony vine residue is the mixture of a kind of in producing juice from Chinese wolfberry, matrimony vine water extract, matrimony vine alcohol extract, LBP-X, Chinese wolfberry fruit wine, fermentation Chinese wolfberry fruit wine, separation matrimony vine seed or producing residue that matrimony vine functional components produces or at least two kinds;

Preferably, described matrimony vine functional component is the mixture of a kind of in wolfberry pigment, matrimony vine flavones, folium lycii flavine, matrimony vine betaine or matrimony vine zeaxanthin or at least two kinds.

3. matrimony vine soluble dietary fiber as claimed in claim 1 or 2, is characterized in that, described soluble dietary fiber, and composition is the mixture of a kind of in pectin, glucan, soluble cellulose or solubility hemicellulose or at least two kinds.

4. the preparation method of the matrimony vine soluble dietary fiber as described in one of as any in claims 1 to 3, is characterized in that, comprise the following steps:

(1) raw material: matrimony vine slag;

(2) extract: the extract adding 5 ~ 35 times of weight in matrimony vine slag, the preferably extract of 10 ~ 20 times of weight, the more preferably extract of 15 times of weight; Soak, then extract, extraction time is 0.5 ~ 10h, preferably 2 ~ 6h, more preferably 2.5h; Separation of Solid and Liquid, collects supernatant;

Wherein, the extract described in step (2) is acid solution or alkali lye;

Preferably, described acid solution is the mixture of any one or at least two kinds in hydrochloric acid, acetic acid, citric acid, malic acid, oxalic acid, sulfuric acid, nitric acid or lactic acid; Acid strength is 0.1% ~ 10%, preferably 0.5 ~ 2%, more preferably 0.7%;

Preferably, described alkali lye is NaOH or KOH; Concentration of lye is 0.5 ~ 10%, preferably 0.5 ~ 3%, more preferably 0.9%.

5. the preparation method of the matrimony vine soluble dietary fiber as described in one of as any in claims 1 to 3, is characterized in that, comprise the following steps:

(1) raw material: matrimony vine slag;

Wherein, the acid solution described in step (2) is any one or at least two or more mixture in hydrochloric acid, acetic acid, citric acid, malic acid, oxalic acid, sulfuric acid, nitric acid or lactic acid; Acid strength is 0.1% ~ 10%, preferably 0.5 ~ 2%, more preferably 0.7%;

Alkali lye described in step (3) is NaOH or KOH; Concentration of lye is 0.5 ~ 10%, preferably 0.5 ~ 3%, more preferably 0.9%.

6. the preparation method of the matrimony vine soluble dietary fiber as described in one of as any in claims 1 to 3, is characterized in that, comprise the following steps:

(1) raw material: matrimony vine slag;

Wherein, the alkali lye described in step (2) is NaOH or KOH; Concentration of lye is 0.5 ~ 15%, preferably 0.5 ~ 3%, more preferably 0.9%;

Acid solution described in step (3) is the mixture of any one or at least two kinds in hydrochloric acid, acetic acid, citric acid, malic acid, oxalic acid, sulfuric acid, nitric acid or lactic acid; Acid strength is 0.1% ~ 10%, preferably 0.5 ~ 2%, more preferably 0.7%.

7. the preparation method of the matrimony vine soluble dietary fiber as described in one of as any in claim 4 ~ 6, is characterized in that, in step (2) or step (3), extracting mode adopts heating to extract or ultrasonic extraction;

Preferably, described heating is extracted, and Extracting temperature remains on 60 ~ 100 DEG C, preferably 80 ~ 90 DEG C, more preferably 85 DEG C; Extraction time 0.5 ~ 3h, preferably 1 ~ 2h, more preferably 1.5h;

Preferably, described ultrasonic extraction, extraction conditions is power 5W ~ 1000W/L, preferred 50W ~ 100W/L, more preferably 80W/L; Extraction time 0.5 ~ 2h, preferably 1 ~ 2h, more preferably 1.5h.

8. the preparation method of the matrimony vine soluble dietary fiber as described in one of as any in claim 4 ~ 6, it is characterized in that, the feed liquid after soaking in step (2) is extracted after pulverizing again;

Preferably, described pulverizing adopts colloid mill to carry out ultramicro grinding or adopts liquid micronizer to pulverize;

Preferably, step (2) or the middle solid-liquid separation method of step (3) adopt a kind of mode in 3-foot solid-liquid separating machine, disc separator, sedimentation centrifuge to carry out;

Preferably, before with alcohol settling, extract adopts acid or alkali to regulate pH value of solution to 6.5 ~ 7.5, and preferred pH7.0, then carries out alcohol settling.

9. the preparation method of the matrimony vine soluble dietary fiber as described in one of as any in claims 1 to 3, is characterized in that, comprise the following steps:

Preferably, the mass ratio of described matrimony vine slag and water is 1:5 ~ 1:30, preferred 1:10 ~ 1:15, more preferably 1:12;

Preferably, the granularity after described pulverizing is 100 ~ 600 orders, preferably 200 ~ 400 orders, more preferably 300 orders;

Preferably, described enzymolysis enzyme is the complex enzyme of a kind of or at least two or more composition in cellulase, hemicellulase, AMS, carbohydrase, arabanase, protease;

Preferably, described hydrolysis temperature is 20 ~ 60 DEG C, preferably 30 ~ 50 DEG C, more preferably 45 DEG C; Enzymolysis time is 0.5 ~ 24h; Preferably 2 ~ 10h, more preferably 3h;

Preferably, described enzyme-removal temperature is 50 ~ 95 DEG C, preferred 80-90 DEG C, more preferably 88 DEG C, and the enzyme time of going out is 2min;

Preferably, described Separation of Solid and Liquid adopts centrifuge to be tripod pendulum type batch centrifugal or horizontal centrifuge; With in described tripod pendulum type batch centrifugal centrifugation step, the order number of filter cloth is 200 ~ 500 orders, preferably 300 orders;

(5) dry: sediment adopts the ethanol of 75 ~ 100% to clean; Drying is carried out to the sediment after washing, dried material is pulverized or grinding, obtains solubility matrimony vine dietary fiber.

10. the preparation method of the matrimony vine soluble dietary fiber as described in one of as any in claim 4 ~ 9, it is characterized in that, the drying mode of the dietary fiber of alcohol settling gained adopts spraying dry, fluidized bed drying or freeze drying to carry out drying;

Wherein, described spraying dry, EAT is 120 ~ 220 DEG C, preferably 150 ~ 190 DEG C, preferably 180 DEG C;

Described fluidized bed drying, baking temperature is 60 ~ 95 DEG C, preferably 70 ~ 80 DEG C, more preferably 75 DEG C.