CN102618599B - Multistage membrane separation purification method of high-purity fructo-oligosaccharide - Google Patents
Multistage membrane separation purification method of high-purity fructo-oligosaccharide Download PDFInfo
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Abstract
The invention relates to a separation purification method of fructose, and especially discloses a multistage membrane separation purification method of high-purity fructo-oligosaccharide. The multistage membrane separation purification method of the high-purity fructo-oligosaccharide is characterized by adopting a fermentation broth and comprising the following steps of 1, carrying out pretreatment on the fermentation broth so that a pH value of the fermentation broth is maintained in a weakly acidic state, 2, adding cane sugar into the fermentation broth treated by the step 1 according to a mass ratio of the fermentation broth to the cane sugar of 1: (0.3 to 0.4) for an enzymatic conversion reaction so that an enzymatic conversion liquid is obtained, 3, removing bacteria and macromolecular substances by membranes through feeding the enzymatic conversion liquid obtained by the step 2 into an inorganic membrane system to obtain a clear fructo-oligosaccharide-containing liquid which does not contain impurities, 4, feeding the clear fructo-oligosaccharide-containing liquid obtained by the step 3 through a multistage organic membrane system to remove impurities and to obtain the high-purity fructo-oligosaccharide, and 5, carrying out decoloration purification, vacuum condensation and drying of the high-purity fructo-oligosaccharide to obtain a finished product of the high-purity fructo-oligosaccharide. The multistage membrane separation purification method of the high-purity fructo-oligosaccharide has advantages that a cost is low; the processes are simple; and the product does not contain impurities.
Description
Technical field
The present invention relates to oligose separation purification method, relate in particular to a kind of separation purification method of oligofructose.
Background technology
Along with the development of world economy and enriching constantly of people's living standard, the nutrient health of food and safety become the focus that people pay close attention to, and the concepts such as " intestinal health " " enteron aisle revolution " " bifidus factor " are constantly proposed and accept by people.As a kind of bifidus factor safely and efficiently, oligofructose is subject to health food development especially persons' favor.
Oligofructose, claims again Nutriflora P or fructooligosaccharide, and molecular formula (G-F-Fn, n=1,2,3, wherein G is glucose, F is fructose).By β-1, the kestose that the fructosyl in 2 glycosidic links and sucrose is combined into, the general name of one group of oligose such as GF3 and GF4 by 1-3 fructosyl.It is extensively present in banana, garlic, and honey, among the foods such as onion.
The physico-chemical property of oligofructose:
1. sugariness and taste matter: the sugariness of the oligofructose that purity is 50%～60% is about 60% of sucrose, the oligofructose sugariness that purity is 95% is approximately only 30% of sucrose, and salubrious compared with sucrose sweet taste, taste is pure, is not with any aftertaste.
1, calorific value: the oligofructose calorific value of in-vivo measurement is only 1.5Kcal/g, and calorific value is extremely low.
2, viscosity: within the scope of 0～70 ° of C, the viscosity with temperature of oligofructose rises and declines, and easily operates during food-processing.
3, moisture content is active: the moisture content of oligofructose is active suitable with sucrose.
4, moisture retention: the moisture retention of oligofructose and sorbyl alcohol, maltose are similar.Be applicable to the long food of moisture preserving time, to guarantee the shelf-lives of food.
5, thermostability: oligofructose is under 120 ° of C neutrallty conditions, and stability and sucrose are close.
6, other processing characteristics solvabilities, non-staining, plastic property, alkali resistance, resistance to deterioration etc. are excellent.
Oligofructose physiological property:
1. in two-ways regulation body, be the eubiosis: promote the rapid propagation of bifidus bacillus, suppress the breeding of putrefactive bacterium in external source pathogenic bacterium and intestines, reduce the pollution of enterogenous endotoxin.
2. relax bowel: promote intestines peristalsis, remove enteron aisle rubbish, prevent constipation, diarrhoea, improve functions of intestines and stomach.Reduce toxic metabolite product, protection liver.
3. regulate blood fat: reduce serum cholesterol.Improve lipid metabolism, improve hypertension, arteriosclerosis, cardiovascular disorder.
4. promote that in human body, vitamin B complex is synthetic: improve body metabolism, strengthening immunity and disease resistance.5. promote mineral absorption: can promote digesting and assimilating of the Grapeseed Oils such as calcium in food, iron, zinc, improve malnutrition, promote to grow and preventing osteoporosis disease.
Also have in addition preventing dental caries, prevent the effects such as fat.
Security: nineteen eighty-two, institute of central authorities of Japanese Meiji Seika Kaisba company has carried out acute toxinology experiment to the security of oligofructose, sub-acute toxicity test, the test-results such as diarrhea test show, oligofructose has security as food and food ingredients.One research group was by methylating afterwards, gas-liquid chromatography (GLC), the analyses of gas chromatography-mass spectrum (coupling) method (GC-MS) and nucleus magnetic resonance (NMR) have drawn the oligofructose GF1 that microorganism fructose-transferring enzyme is produced, GF2, the chemical structural formula of GF3, and clear and definite its mechanism of action.
On November 22nd, 2000, U.S. FDA is formally using oligofructose (FOS) as generally recognized as safe level (GRAS) functional food ingredient, and this is first functional oligose of formally examining by FDA up to now.
As can be seen here, oligofructose is a kind of food of security, meets the intension of third generation protective foods completely.
Application:
1, as probiotics, be bifidus bacillus regulator.Not only can make the function of product affix oligofructose, and can overcome some defect of original product, make product more perfect.As at interpolation oligofructoses such as grain productss, can obtain high product quality and extend the product shelf phase.
2, as dietary cellulose, can effectively reduce serum cholesterol and blood fat, to the hypertension causing because blood fat is high, arteriosclerosis etc., there are a series of cardiovascular disordeies to have a better role.
3, as activation factor, be the activation factor of the mineral substance such as calcium, magnesium, iron and trace element, can reach the effect that promotes mineral substance and absorption of trace elements.
4, as nutrient substance, can promote naturally synthetic category-B vitamin complex in body, there is the effect of supporting that brain, neural system, digestion and energy generate.
CN 10137690 A announce a kind of production method of high-purity fructo oligosaccharides, the method is placed in film enzyme reactor by oligofructose raw material, under the effect of enzyme, make disaccharides be converted into oligofructose and monose, monose sees through film and filtering, thereby obtains the oligofructose that purity is greater than 95%; The method need to adopt membrane reactor, and operational requirement is high.CN 101289681 A announce a kind of production method of high-purity fructo oligosaccharides, it is raw material that the method be take 55% regular grade oligofructose, utilize bio-transformation principle, adopt yeast conversion to eliminate the glucose in common oligofructose, oligofructose content is reached more than 75%, the separation of recycling ion-exchange chromatography and membrane separation technique combine, and remove other compositions, make the oligofructose content in product be greater than 95%.This method needs oligofructose that concentration is higher as raw material, by yeast, ion-exchange chromatography, membrane separation technique, is used in combination to obtain purity oligofructose, but the step of separation and purification is more, the efficiency that is difficult to guarantee separation and purification.
Summary of the invention
The present invention is intended to address the aforementioned drawbacks, and a kind of separation purification method of Using Multistage Membranes system of high-purity fructo oligosaccharides is provided.Method of the present invention is with low cost, and working method is simple, and product is free from foreign meter.
The present invention is achieved in that a kind of Using Multistage Membranes separation purification method of high-purity fructo oligosaccharides, and it comprises the fermented liquid of use; And comprise the following steps:
Step a, fermentation liquor pretreatment, makes its pH value remain on slightly acidic;
Step b, carries out enzymatic conversion reaction in the fermented liquid that adds step a to process sucrose obtain enzymatic conversion liquid according to the ratio of the mass ratio 1:0.3-0.4 of fermented liquid and sucrose;
Step c, film removes thalline and macromolecular substance: the enzymatic conversion liquid that step b is obtained enters mineral membrane system, the clear liquid containing oligofructose of the impurity that is removed, working pressure 0.1-0.3Mpa, temperature 40-50 ℃; Mode by moisturizing in process improves product yield;
Steps d, the described clear liquid that step c is obtained, by multistage organic membrane system, is removed impurity, obtains high-purity fructo oligosaccharides liquid, and pressure-controlling is at 1.5-2.5Mpa, temperature 35-45 ℃; Mode by moisturizing in process reaches deimpurity object;
Step e, by described high-purity fructo oligosaccharides decolouring removal of impurities, vacuum concentration and drying operation, obtains high-purity fructo oligosaccharides.
The multistage organic membrane separation purification method of described high-purity fructo oligosaccharides, described fermented liquid is: a kind of fermented liquid that contains fructosyl transferase.
The multistage organic membrane separation purification method of described high-purity fructo oligosaccharides, the pH value of the fermented liquid of described step a is 5-7.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, in described steps d, Using Multistage Membranes system is organic membrane, and progression is 4-9 level, and membrane module molecular weight cut-offs at different levels are 5000-300D.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, in described steps d, multistage continuous film system feeding concentration is defined as 2-25% according to oligofructose and monose, assorted sugared content (wt%) in enzymatic conversion liquid, discharge concentration is monosaccharide concentration and oligofructose concentration, is 5-30%.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, in described step e, described removal of impurities operation adopts powdered carbon or granulated active carbon, and vacuum concentration is used short-path distillation equipment.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, two steps of c and d can be carried out continuous coupled or operation separately, and wherein, the membrane pore size that step c is used is 50-500nm.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, the membrane material of described step c is mineral membrane.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, the membrane material of described step c is stainless steel membrane.
The present invention utilizes fermented liquid directly sucrose to be transformed, and utilizes mineral membrane system and organic Using Multistage Membranes system to remove impurity, purifying oligofructose product, and working method is very simple, without using enzyme mebrane reactor, with low cost, and in product, does not contain impurity.
embodiment
Below, in conjunction with embodiment, the present invention is described further:
A Using Multistage Membranes separation purification method, it comprises the fermented liquid of use; And comprise the following steps:
Step a, fermentation liquor pretreatment, makes its pH value remain on slightly acidic;
Step b, carries out enzymatic conversion reaction in the fermented liquid that adds step a to process sucrose obtain enzymatic conversion liquid according to the ratio of the mass ratio 1:0.3-0.4 of fermented liquid and sucrose;
Step c, film removes thalline and macromolecular substance: the enzymatic conversion liquid that step b is obtained enters film system, the clear liquid containing oligofructose of the impurity that is removed, working pressure 0.1-0.3Mpa, temperature 40-50 ℃; Mode by moisturizing in process improves product yield;
Steps d, the described clear liquid that step c is obtained, by Using Multistage Membranes system, is removed impurity, obtains high-purity fructo oligosaccharides liquid, and pressure-controlling is at 1.5-2.5Mpa, temperature 35-45 ℃; Mode by moisturizing in process reaches deimpurity object;
Step e, by described high-purity fructo oligosaccharides decolouring removal of impurities, vacuum concentration and drying operation, obtains high-purity fructo oligosaccharides.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, described fermented liquid is: a kind of fermented liquid that contains fructosyl transferase.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, the pH value of the fermented liquid of described step a is 5-7.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, in described steps d, Using Multistage Membranes system is organic membrane, and progression is 4-9 level, and membrane module molecular weight cut-offs at different levels are 5000-300D.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, in described steps d, multistage continuous film system feeding concentration is defined as 2-25% according to oligofructose and monose, assorted sugared content (wt%) in enzymatic conversion liquid, discharge concentration is monosaccharide concentration and oligofructose concentration, is 5-30%.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, in described step e, described removal of impurities operation adopts powdered carbon or granulated active carbon, and vacuum concentration is used short-path distillation equipment.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, two steps of c and d can be carried out continuous coupled or operation separately, and wherein, the membrane pore size that step c is used is 50-500nm.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, the membrane material of described step c is mineral membrane.
The Using Multistage Membranes separation purification method of described high-purity fructo oligosaccharides, the membrane material of described step c is stainless steel membrane.
Embodiment 1:
Get 55kg fermented liquid, after pre-treatment, add wherein sucrose 20kg sucrose to carry out enzymatic conversion reaction, reacting rear material enters removal of impurities film system, and film system is inorganic stainless steel membrane system, aperture 100 nanometers, process temperature is controlled 35-45 ℃, and 0.6 square metre of membrane area, obtained cleaner liquid 112kg; Clear liquid enters 6 grades of organic membrane separation systems, and operating pressure is controlled at 1.8Mpa, temperature 35-40 ℃, and dope side obtains material 92kg, oligofructose purity 98%, oligofructose content 135g/L.
Embodiment 2:
Get 40kg fermented liquid, after pre-treatment, add wherein sucrose 13kg sucrose to carry out enzymatic conversion reaction, material enters removal of impurities film system, uses 0.2 square metre of mineral membrane area, membrane pore size 50 nanometers, enter film pressure 0.3Mpa, go out film pressure 0.22Mpa, process temperature is controlled 40 ℃, obtains cleaner liquid 83kg; Clear liquid enters 5 grades of film separating systems, and system pressure is controlled at 1.8-2.0Mpa, 38 ℃ of service temperatures, and dope side obtains material 68kg, oligofructose purity 96.5%, oligofructose content 118g/L.
The 250kg obtaining through 6 grades of film separating systems in embodiment 1 sees through clear liquid and obtains 25kg concentrated solution through vacuum concentration operation, sugar concentration 32%, dope side material, through the removal of impurities of powder activity carbon decoloring, obtains transparent liquid, again through the concentrated product, product purity 98% of obtaining of short-path distillation; The 68kg dope that embodiment 2 obtains through 5 grades of film separating systems obtains product white powder, product purity 96.5% through decolorizing with activated carbon, vacuum concentration and spray thing drying treatment.
Claims (6)
1. a Using Multistage Membranes separation purification method for high-purity fructo oligosaccharides, is characterized in that, it comprises the fermented liquid of use; And comprise the following steps:
Step a, fermentation liquor pretreatment, makes its pH value remain on slightly acidic; Described fermented liquid is: a kind of fermented liquid that contains fructosyl transferase, and enzyme concn is every hectogram 100-200 unit;
Step b, carries out enzymatic conversion reaction in the fermented liquid that adds step a to process sucrose obtain enzymatic conversion liquid according to the ratio of the mass ratio 1:0.3-0.4 of fermented liquid and sucrose;
Step c, film removes thalline and macromolecular substance: the enzymatic conversion liquid that step b is obtained enters mineral membrane system, the clear liquid containing oligofructose of the impurity that is removed, working pressure 0.1-0.3MPa, temperature 40-50 ℃, the mode by moisturizing in process improves product yield; The mineral membrane aperture of using is 50-500nm;
Steps d, the described clear liquid that step c is obtained enters multistage organic membrane system, removes impurity, obtains high-purity fructo oligosaccharides liquid, and pressure-controlling is at 1.5-2.5MPa, temperature 35-45 ℃, and the mode by moisturizing in process reaches deimpurity object; The progression of described multistage organic membrane system is 4-9 level, and membrane module molecular weight cut-offs at different levels are 5000-300D;
Step e, by described high-purity fructo oligosaccharides liquid decolour removal of impurities, vacuum concentration and drying operation, obtains high-purity fructo oligosaccharides.
2. the Using Multistage Membranes separation purification method of high-purity fructo oligosaccharides according to claim 1, is characterized in that, the pH value of the fermented liquid of described step a is 5-7.
3. the Using Multistage Membranes separation purification method of high-purity fructo oligosaccharides according to claim 1, it is characterized in that, in described steps d, multistage organic membrane system input concentration is defined as 2-25% according to oligofructose and monose, assorted sugared content in enzymatic conversion liquid, discharge concentration is monosaccharide concentration and oligofructose concentration, for 5-30%, described percentage ratio is all weight percentage.
4. the Using Multistage Membranes separation purification method of high-purity fructo oligosaccharides according to claim 1, is characterized in that, in described step e, described removal of impurities operation adopts powdered carbon or granulated active carbon, and vacuum concentration is used short-path distillation equipment.
5. the Using Multistage Membranes separation purification method of high-purity fructo oligosaccharides according to claim 1, is characterized in that: step c and d can carry out continuous coupled or operation separately.
6. the Using Multistage Membranes separation purification method of high-purity fructo oligosaccharides according to claim 1, is characterized in that, the mineral membrane material of described step c is stainless steel membrane.
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