CN115109810A - Fructo-oligosaccharide and preparation method thereof - Google Patents

Fructo-oligosaccharide and preparation method thereof Download PDF

Info

Publication number
CN115109810A
CN115109810A CN202210867137.1A CN202210867137A CN115109810A CN 115109810 A CN115109810 A CN 115109810A CN 202210867137 A CN202210867137 A CN 202210867137A CN 115109810 A CN115109810 A CN 115109810A
Authority
CN
China
Prior art keywords
fructo
oligosaccharide
glucose
sucrose
dry basis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202210867137.1A
Other languages
Chinese (zh)
Inventor
金建国
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN202210867137.1A priority Critical patent/CN115109810A/en
Publication of CN115109810A publication Critical patent/CN115109810A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/04Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/52Adding ingredients
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/125Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives containing carbohydrate syrups; containing sugars; containing sugar alcohols; containing starch hydrolysates
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/20Reducing nutritive value; Dietetic products with reduced nutritive value
    • A23L33/21Addition of substantially indigestible substances, e.g. dietary fibres
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/18Preparation of compounds containing saccharide radicals produced by the action of a glycosyl transferase, e.g. alpha-, beta- or gamma-cyclodextrins
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/24Preparation of compounds containing saccharide radicals produced by the action of an isomerase, e.g. fructose
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Zoology (AREA)
  • Wood Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Biochemistry (AREA)
  • Biotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Genetics & Genomics (AREA)
  • General Health & Medical Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Nutrition Science (AREA)
  • Polymers & Plastics (AREA)
  • Mycology (AREA)
  • Molecular Biology (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

The invention provides a preparation method of fructo-oligosaccharide, which comprises the steps of treating a sugar source by adopting a complex enzyme; optionally, the method further comprises the step of purifying; the compound enzyme is a mixture of glucose isomerase and beta-fructosyltransferase; the sugar source is rich in sucrose, such as sucrose, sugarcane juice, brown sugar, etc. The invention also provides fructo-oligosaccharide prepared according to the method. The preparation method has high raw material utilization rate which can reach 100% theoretically, and the obtained by-product can be recycled to be completely generated into fructo-oligosaccharide, so that the preparation method is more environment-friendly and economical. In addition, the preparation method can also obtain fructo-oligosaccharide with the purity of more than 90 percent and a corresponding byproduct, namely high fructose syrup, through a purification process, is suitable for industrial production, and can be widely applied to food or health care products.

Description

Fructo-oligosaccharide and preparation method thereof
Technical Field
The invention relates to fructo-oligosaccharide and a preparation method thereof.
Background
Fructooligosaccharides (FOS) are linear oligosaccharides formed from fructosyl glucose and have two forms of structure: one is formed by connecting 1-8 fructosyl groups on fructose residues of sucrose molecules through beta (2-1) glycosidic bonds, the structural formula is represented as GF2-GF9(G is glucosyl group, F is fructosyl group), and fructo-oligosaccharide molecules generated under the conventional conditions are GF2-GF5 (namely, 3 to 6 sugars of sucrose, mainly 3 and 4 sugars of sucrose, 5 sugars of sucrose and 6 sugars of sucrose are extremely little); the other is formed by connecting 3-9 fructose residues through beta (2-1) glycosidic bonds, and the structural formula of the other is represented as F3-F9.
Fructo-oligosaccharide is a natural active substance, has novel sweetening agents with health care functions of regulating intestinal flora, proliferating bifidobacteria, promoting calcium absorption, regulating blood fat, regulating immunity, resisting decayed teeth and the like, and is known as a new generation additive with the most potential after the age of antibiotics, namely a growth promoting substance. The fructo-oligosaccharide has good health promotion effect, is nontoxic, is suitable for diabetic patients, and can be used for preventing dental caries, regulating lipid metabolism, promoting calcium absorption, reducing serum cholesterol, and inhibiting cancer; and can be used as proliferation factor of Bacillus bifidus to improve disease resistance and immunity of human body; because the fructo-oligosaccharide has the function of water-soluble dietary fiber, the fructo-oligosaccharide can be used as a rheology and tissue modifier, a water retention agent and the like to be widely applied to low-calorie food and beverages, dietary fiber or prebiotics food and beverages, and can also be applied to common food and beverages.
In the prior art, fructosyl transferase is mostly adopted to hydrolyze and polymerize sucrose into fructo-oligosaccharide, theoretically, 100 g of sucrose generates 75% of fructo-oligosaccharide (pure fructo-oligosaccharide trisaccharide) at most, namely, 1 sucrose molecule and one fructose molecule are polymerized into fructo-oligosaccharide, namely, 50 g of sucrose and 25 g of fructose polymerize into 75 g of fructo-oligosaccharide, and the rest 25 g of glucose is waste, but in the actual production process, 100 g of sucrose can only generate 50-60 g of fructo-oligosaccharide, even after two purifications (the first chromatographic purification is used for extracting the fructo-oligosaccharide part, and the second chromatographic purification is used for extracting the monosaccharide part, namely glucose and fructose) in the later period, the purified residual liquid is fermented again, and the yield of the fructo-oligosaccharide is difficult to reach 75%, and is generally maintained within 60%.
Disclosure of Invention
The first aspect of the invention aims to provide a method for preparing fructo-oligosaccharide, which comprises the step of treating a sugar source by adopting complex enzyme; optionally, the method further comprises the step of purifying; the compound enzyme is a mixture of glucose isomerase and beta-fructosyltransferase; the sugar source is rich in sucrose, such as sucrose, beet juice, sugarcane juice, brown sugar, etc. Preferably, the glucose isomerase and beta-fructosyltransferase are used non-simultaneously.
In one or more embodiments, at least one of the complex enzymes is an immobilized enzyme.
In one or more embodiments, the ratio of enzyme activity, glucose isomerase: beta-fructosyltransferase > 1:2, preferably 1: 1.
The proportion of the glucose isomerase is adjusted according to different requirements, and the higher the proportion of the glucose isomerase is, the higher the fructose content is, and the lower the glucose content is.
In one or more embodiments, the purification step is chromatographic purification, nanofiltration, microfiltration or ultrafiltration.
In one or more embodiments, the byproduct obtained after purifying the complex enzyme and sugar source reaction product is used as a sugar source to continue the reaction.
The product is herein referred to as by-product 1, by-product 1 being a high fructose syrup rich in fructooligosaccharides (fructooligosaccharides greater than 20% (on a dry basis), fructose greater than 30% (on a dry basis), sucrose greater than 30% (on a dry basis).
In one or more embodiments, the method further comprises a step of performing secondary purification on the byproduct, and continuing to react the secondary purified substances except the high fructose syrup as a sugar source.
The by-products include by-product 2 and by-product 3, wherein the by-product 2 is high fructose syrup with fructose content more than 60% (dry basis); the by-product 3 is a mixture of FOS and sucrose, the content of the FOS is more than 30% (dry basis), and the content of the sucrose is more than 30% (dry basis).
And (3) performing complex enzyme fermentation on the byproduct 1 and the byproduct 3 again to obtain a fructo-oligosaccharide product with the purity of fructo-oligosaccharide of more than 50 percent, wherein the fructo-oligosaccharide is the polymerization of sucrose and fructose, and theoretically, all the sucrose can be completely reacted into the fructo-oligosaccharide by repeating the steps.
In the actual production process, the generation amount of the byproduct 1 and the byproduct 3 is often not controlled, sometimes more or less, at this time, the raw material syrup with any content (such as cane syrup, sugarcane concentrated juice, red syrup and the like) can be mixed, then fermentation is carried out, and an oligofructose product with the purity of oligofructose of more than 50 percent can be obtained as well.
In one or more embodiments, the process further comprises a post-treatment step of concentrating or drying the resulting fructooligosaccharides.
The fructo-oligosaccharide pulp product and the byproduct high fructose syrup product generated by the invention generally need to be concentrated or dried, can be stored at normal temperature, and have the same production process as the prior fructo-oligosaccharide or high fructose syrup production process.
The second aspect of the present invention aims to provide a fructooligosaccharide obtained by any one of the preparation methods of the present invention, wherein the fructooligosaccharide has one or more of the following characteristics:
the yield of fructo-oligosaccharide obtained by the method without purification is more than 50 percent (accounting for dry basis);
the purity of the fructo-oligosaccharide obtained by the method after purification is more than 90 percent (on a dry basis).
In addition, the fructose oligosaccharide obtained by the invention has reduced sugar-rising component (glucose content); the fructo-oligosaccharide has no sugar component (fructose content) increase.
The third aspect of the invention aims to provide the application of the fructo-oligosaccharide in food, wherein the food is low-calorie food and beverage, dietary fiber or prebiotics food and beverage, and can also be used in common food and beverage.
The fourth aspect of the present invention is to provide the use of said fructo-oligosaccharide in health products or health foods, which has the effect of controlling blood sugar. The health product may be a low GI beverage (glucose content or raw material content for glucose production by enzymatic hydrolysis with human digestive enzymes is controlled, in this patent sucrose (1 g sucrose can produce 0.5 g glucose), glucose is the main ingredient). The fructose and the fructo-oligosaccharide do not generate glucose so as not to cause the rise of blood sugar, and glucose molecules do not need to be decomposed and directly enter blood to cause the rise of the blood sugar of a human body.
Compared with the prior art, the preparation method is simple, the utilization rate of the raw materials is high (the repeated recovery fermentation can reach 100 percent), the obtained by-products can be repeatedly utilized and fermented again, and the method is more environment-friendly and economical. In addition, the preparation method can obtain fructo-oligosaccharide with the purity of more than 90 percent, is suitable for industrial production, and can be widely applied to food or health care products.
Drawings
FIG. 1 shows the preparation of fructo-oligosaccharides described in the examples (purification by chromatography followed by fermentation of by-product 1 to give fructo-oligosaccharides).
FIG. 2 shows the preparation of fructo-oligosaccharide described in the examples (two chromatographies to obtain by-product 2-high fructose syrup, and by-product 3 is fermented again to produce fructo-oligosaccharide).
Detailed Description
The present invention will be described in detail below. The technical features described below are explained based on typical embodiments and specific examples of the present invention, but the present invention is not limited to these embodiments and specific examples. It should be noted that:
it is to be understood that within the scope of the present invention, the above-described technical features of the present invention and the technical features described in detail below (e.g., the embodiments) may be combined with each other to constitute a preferred embodiment.
To make the features and effects of the present invention comprehensible to those skilled in the art, general description and definitions are made below with reference to terms and expressions mentioned in the specification and claims. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The theory or mechanism described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features defined herein as numerical ranges or percentage ranges, such as values, amounts, levels and concentrations, are for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to cover and specifically disclose all possible subranges and individual numerical values (including integers and fractions) within the range. Herein, the percentage refers to a mass percentage unless otherwise specified.
In this context, for the sake of brevity, not all possible combinations of features in the various embodiments or examples are described. Therefore, the respective features in the respective embodiments or examples may be arbitrarily combined as long as there is no contradiction between the combinations of the features, and all the possible combinations should be considered as the scope of the present specification.
The preparation process of the present invention is further described in detail with reference to the following specific embodiments and examples. It should be understood that these detailed description and examples are illustrative only and are not intended to limit the scope of the invention.
In the following examples, the beta-fructosyltransferase used was purchased from Henan Sanhua Biotech Ltd; the adopted glucose isomerase is purchased from Henan Huayue chemical products, Inc., and is immobilized enzyme.
In the following examples, measurement methods of fructooligosaccharide, sucrose, fructose and glucose were measured by the method described in the national standard (GB/T23528.2).
The preparation method of fructo-oligosaccharide adopted in the following examples is shown in figure 1, and specifically comprises the following steps:
(1) preparing a sugar source, and adding a complex enzyme consisting of glucose isomerase and beta-fructosyltransferase; according to the enzyme activity ratio, glucose isomerase: beta-fructosyltransferase > 1: 2;
(2) purifying the reaction product of the sugar source and the compound enzyme, wherein the purification step is chromatographic purification, nanofiltration, microfiltration or ultrafiltration;
(3) as shown in figure 1, after purification, fructo-oligosaccharide with content of more than 50% (dry basis) and byproduct 1 are obtained, wherein byproduct 1 is high fructose syrup rich in fructo-oligosaccharide (fructo-oligosaccharide is more than 20% (dry basis), fructose is more than 30% (dry basis), and sucrose is more than 30% (dry basis)); purifying the reaction product of the complex enzyme and the sugar source to obtain a byproduct, and taking the byproduct as the sugar source to continue the reaction;
(4) concentrating or drying the separated fructo-oligosaccharide.
The preparation method of fructo-oligosaccharide adopted in the following examples can also be shown in fig. 2, and the preparation method further comprises a step of performing secondary purification on the byproduct 1, and the specific steps are as follows:
(1) preparing a sugar source, and adding a complex enzyme consisting of glucose isomerase and beta-fructosyltransferase; according to the enzyme activity ratio, glucose isomerase: beta-fructosyltransferase > 1: 2;
(2) purifying the reaction product of the sugar source and the complex enzyme, wherein the purification step is chromatographic purification, nanofiltration, microfiltration or ultrafiltration;
(3) as shown in figure 1, after purification, fructo-oligosaccharide with content of more than 50% (dry basis) and byproduct 1 are obtained, wherein byproduct 1 is high fructose syrup rich in fructo-oligosaccharide (fructo-oligosaccharide is more than 20% (dry basis), fructose is more than 30% (dry basis), and sucrose is more than 30% (dry basis));
(4) purifying the byproduct 1 to obtain a byproduct 2 and a byproduct 3, wherein the byproduct 2 is high fructose syrup, and the fructose content of the byproduct is more than 60% (dry basis); the byproduct 3 is a mixture of FOS and sucrose, the content of the FOS is more than 30% (dry basis), and the content of the sucrose is more than 30% (dry basis); taking the other substances except the high fructose syrup after the secondary purification as sugar sources to continue reacting;
(5) concentrating or drying the separated fructo-oligosaccharide.
Both of the above-mentioned methods involve the preparation of the same fructooligosaccharide fermentation broth: weighing white granulated sugar, adding water to dissolve, fermenting at 50 ℃ by using an immobilized enzyme method, and stopping fermentation when monitored data meet requirements to obtain fructo-oligosaccharide fermentation liquor; the fermentation liquor has low glucose content, high fructose content, and sweetness higher than that of fructo-oligosaccharide product produced by conventional fermentation, and is also beneficial to reducing glucose intake for people.
1. Examples 1 to 3 and comparative example
The amounts of raw materials and reaction conditions specifically added in examples 1 to 3 and comparative example are shown in Table 1;
table 1: summary of the amounts of raw materials added and reaction conditions for examples 1-3 and comparative examples
Figure BDA0003759796400000061
Sugar degree of syrup: 50-60% (can be detected by sugar degree instrument, namely dry solid or soluble solid)
Fermentation temperature: 50-60 degrees
Fermentation pH: 5.0-7.0
Comparative example:
the specific amounts of the raw materials added and the reaction conditions in the comparative example are shown in Table 2;
table 2: amount of raw materials added in comparative example, reaction conditions
Figure BDA0003759796400000071
Sugar degree of syrup: 50-60% (can be detected by sugar degree instrument, namely dry solid or soluble solid)
Fermentation temperature: 50-60 degrees
Fermentation pH: 5.0-7.0
Note: the enzyme activities of the fructosyltransferase and glucose isomerase raw materials are not limited, the addition amount is not limited, the main reason is that the enzyme activities and forms of different manufacturers are different, the fructosyltransferase (immobilized enzyme) and glucose isomerase (immobilized enzyme) are mixed and fermented in the test, the enzyme activities of the fructosyltransferase and glucose isomerase (immobilized enzyme) are both about 100u/g, and in the using process of the embodiment and the comparative example, about 650 g of immobilized fructosyltransferase is added into 5 kg of sucrose, so that 5 kg of sucrose can be converted into fructo-oligosaccharide syrup with fructooligosaccharide accounting for more than 50% (dry basis) in 4 hours.
The addition amount of fructosyltransferase is not particularly limited, but generally, it is desirable that the fermentation time is short, that fructosyltransferase can be added in a large amount, that the fermentation time is controlled to 3.5 to 4.5 hours, that the time is shortened, that the addition amount of enzyme can be increased, that the time is allowed to be longer, that the addition amount of enzyme can be appropriately reduced, and that the time calculation method is as follows:
such as fructosyltransferase, 12u enzyme activity, under appropriate conditions, 1 gram of granulated sugar can be converted into fructo-oligosaccharide (on a dry basis) with a concentration of more than about 50% in 4 hours.
Glucose isomerase, 12u enzyme activity, can convert 1 g of glucose into fructose (accounting for dry basis) with a content of more than 50% in 4 hours under the conditions of pH and temperature suitable for fructosyltransferase.
The fructosyltransferase is expensive, attention needs to be paid to control during addition, glucose isomerase is cheap and is suitable for being added in more amount, and the higher the addition amount is, the lower the glucose content in the fermentation liquor is, the lower the glucose content is, the fructosyltransferase is generally controlled to be 0.5-2 times of the enzyme activity of the fructosyltransferase, but the fructosyltransferase is not particularly limited.
Determination of the activity of the glucose isomerase: the enzyme activity of the glucose isomerase is determined again under the condition that fructosyl transferase is suitable for fermenting sucrose to generate fructo-oligosaccharide (such as pH5-7 and temperature 50-60 ℃), and the most suitable pH and temperature of the glucose isomerase are not completely in the range, so the most suitable pH and temperature is generally 7.0-7.5 and the temperature is generally within 60 ℃.
But the cost is low, the addition amount can be properly increased to be matched with the fermentation of glucose to generate fructose, and the enzyme activity can be re-detected at the pH and temperature suitable for the fermentation of fructosyltransferase, so that the specific enzyme activity in the test and production process is realized.
Glucose is derived from the decomposition reaction when fructosyltransferase ferments sucrose, one molecule of sucrose generates one molecule of glucose and one molecule of fructose, one molecule of fructose is connected with sucrose or fructo-oligosaccharide to become kestose or nystose, kestopentasaccharide and kestohexasaccharide, and glucose remains in the fermentation liquor. The fructose is reacted by glucose isomerase to produce fructose, which can continuously participate in the reaction process of producing fructo-oligosaccharide.
The detection result of the fructo-oligosaccharide fermentation liquor is as follows:
case(s) Fructose% (on a dry basis) Glucose% (dry basis) Sucrose% (on a dry basis) Fructo-oligosaccharide% (on a dry basis)
Example 1 23.52% 1.68% 16.90% 57.90%
Example 2 18.59% 8.31% 15.80% 57.30%
Example 3 11.20% 13.60% 17.30% 57.90%
Comparative example 3.22% 23.98% 16.50% 56.30%
The sweetness value of the fermentation liquor and the glucose yield after digestion are as follows:
Figure BDA0003759796400000081
Figure BDA0003759796400000091
and (3) sweetness calculation: the total sweetness of the dry base is calculated by taking the sweetness of sucrose as 1, the sweetness of glucose as 0.7, the sweetness of fructose as 1.8 and the sweetness of fructo-oligosaccharide as 0.3,
sucrose to (dry basis) × 1+ glucose to (dry basis) × 0.7+ fructose to (dry basis) × 1.8+ fructo oligosaccharide to (dry basis) × 0.3
Calculation of glucose production: the human body can digest one molecule of sucrose into one molecule of fructose and one molecule of glucose, the fructose can not cause the rise of blood sugar, and meanwhile, the human body digestive juice can not digest fructo-oligosaccharide.
2. Preparation of high-purity fructo-oligosaccharide liquid
And (2) filtering the fructo-oligosaccharide fermentation liquor obtained in the step (1), collecting filtrate, purifying by chromatography, and monitoring that the fructo-oligosaccharide in the purified product accounts for more than 90% (on a dry basis), so as to obtain the fructo-oligosaccharide high-purity liquor and generate a byproduct 1.
Figure BDA0003759796400000092
3. A high fructose syrup (fructose accounts for more than 60% (dry basis)) and an oligofructose syrup (with oligofructose purity of above Preparation of more than 50% (on a dry basis) (FIG. 2)
And (3) performing chromatographic purification for the 2 nd time on the byproduct 1, and emphatically separating monosaccharide components in the byproduct 1 to obtain a byproduct 2: high fructose syrup with fructose content over 60% (on dry basis); and the obtained by-product 3 (fructo-oligosaccharide accounts for more than 30 percent, and sucrose accounts for more than 30 percent) can be directly fermented again to obtain fructo-oligosaccharide syrup with the purity of more than 50 percent, and all products can be utilized by repeating the steps of 1-2-3. Namely, a high-purity fructo-oligosaccharide product (the purity is more than 90 percent (accounting for dry basis)) and a high-purity fructose product (the purity is more than 60 percent (accounting for dry basis)) are generated.
The 1 st chromatographic purification emphasizes the purification of fructo-oligosaccharide products to ensure that the content of the fructo-oligosaccharide reaches more than 90 percent (accounting for dry basis), and the 2 nd chromatographic purification emphasizes the purification of two groups of monosaccharide components of fructose and glucose to ensure that the content of (glucose + fructose) is more than 80 percent (accounting for dry basis). The purpose of the two chromatographic purifications is different.
The produced fructo-oligosaccharide syrup meets the requirements of GB23528.2, can be directly used as fructo-oligosaccharide raw material or prepared into high-purity fructo-oligosaccharide after primary chromatographic purification. After the first chromatographic purification, the high-purity fructo-oligosaccharide is prepared.
Figure BDA0003759796400000101
Sweetness and glucose production comparison of examples to controls:
Figure BDA0003759796400000102
in the comparison example, the compound enzyme fermentation is not adopted, so the produced syrup takes glucose as a main component, the sweetness is low, and the glucose is easy to cause the rise of blood sugar and is not suitable for producing foods for controlling the generation of blood sugar, such as special foods for diabetics or people with high blood sugar.
4. The by-product 1 was fermented again (FIG. 1)
By secondary fermentation, the fructo-oligosaccharide product with the purity of more than 50 percent (calculated by dry basis) can be generated, the process can also be carried out by properly supplementing any amount of sucrose syrup (the supplementing amount is not limited), and the product can be purified by chromatography again to obtain a new byproduct 1. Repeating the steps 1-2-4 to completely convert the sucrose into a high-purity fructo-oligosaccharide product.
In the comparative example, the glucose content in the by-product 1 was too high to affect the action of fructosyltransferase, and the fermentation could not be continued efficiently to produce fructooligosaccharides (to make fructooligosaccharides more than 50% (dry basis)), so the fermentation test was not conducted in (4).
The fructo-oligosaccharide product with the purity of more than 50 percent (calculated by dry basis) can be generated, the process can also be carried out by properly supplementing any amount of sucrose syrup (the supplementing amount is not limited), and the product can be purified by chromatography again to obtain a new byproduct 1. Repeating the steps 1-2-4 to completely convert the sucrose into a high-purity fructo-oligosaccharide product.
Note: the byproduct 1 can be directly used as a raw material for food industry, and the byproduct 1 can be fermented again to generate fructo-oligosaccharide fermentation liquor.
Figure BDA0003759796400000111
In the comparative example, the glucose content of the byproduct 1 is too high, the fructo-oligosaccharide content is low, the sucrose content is insufficient, the continuous fermentation is difficult to generate the fructo-oligosaccharide product with the purity of more than 50 percent, and the fermentation significance is not great, so the fermentation is not carried out. For example, 32.95% of sucrose produces up to 16% of fructo-oligosaccharide (in the limit case), and 25.66% (existing in the byproduct 1), together with about 41% (dry basis), the fructo-oligosaccharide cannot reach the content requirement of over 50% of the fructo-oligosaccharide required by the national standard, so it is meaningless.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. The preparation method of fructo-oligosaccharide is characterized by comprising the step of treating a sugar source by adopting complex enzyme; optionally, the method further comprises the step of purifying; the compound enzyme is a mixture of glucose isomerase and beta-fructosyltransferase; the sugar source is a sugar source rich in sucrose; preferably, the glucose isomerase and beta-fructosyltransferase are also used non-simultaneously, e.g. according to a fermentation process fructooligosaccharides may be prepared and then glucose isomerase may be used to convert the glucose in the by-product to fructose.
2. The process according to claim 1, wherein at least one of the complex enzymes is an immobilized enzyme.
3. The method according to claim 1, wherein the ratio of the enzyme activity of glucose isomerase: beta-fructosyltransferase > 1:2, preferably 1: 1.
4. The method of claim 1, wherein the purification step is chromatographic purification, nanofiltration, microfiltration or ultrafiltration.
5. The preparation method of claim 1, wherein a byproduct obtained by purifying the reaction product of the complex enzyme and the sugar source is used as the sugar source to continue the reaction.
6. The method of claim 5, further comprising a step of secondary purification of the by-product, and further comprising the step of continuing the reaction of the secondary purified materials except for the high fructose syrup as a sugar source.
7. The method of claim 1, further comprising a post-treatment step of concentrating or drying the resulting fructooligosaccharides.
8. An oligofructose obtainable by the process according to any one of claims 1 to 7, said oligofructose having one or more of the following characteristics:
the yield of fructo-oligosaccharide obtained by the method without purification is more than 50 percent (accounting for dry basis);
the purity of the fructo-oligosaccharide obtained by the method after purification is more than 90 percent (on a dry basis).
9. Use of the fructooligosaccharide according to claim 8 in food products, wherein the food products are low-calorie food and beverages, dietary fiber or prebiotic food and beverages, and also in general food and beverages.
10. The use of the fructooligosaccharide according to claim 8 in a health product or health food, which has a blood glucose controlling effect due to a low glucose content and a corresponding decrease in sucrose content (one gram of sucrose can be digested into 0.5 gram of glucose and 0.5 gram of fructose by the human body), said health product being a low GI beverage. Meanwhile, the conventional fructo-oligosaccharide (the fructo-oligosaccharide is more than 50 percent (accounting for dry basis)) produced by the technology has the sweetness of 0.1-0.4 (accounting for dry basis) than that of the common fructo-oligosaccharide (the fructo-oligosaccharide is more than 50 percent (accounting for dry basis)), so that the requirement of people on sweetness is better met.
CN202210867137.1A 2022-07-22 2022-07-22 Fructo-oligosaccharide and preparation method thereof Pending CN115109810A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210867137.1A CN115109810A (en) 2022-07-22 2022-07-22 Fructo-oligosaccharide and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210867137.1A CN115109810A (en) 2022-07-22 2022-07-22 Fructo-oligosaccharide and preparation method thereof

Publications (1)

Publication Number Publication Date
CN115109810A true CN115109810A (en) 2022-09-27

Family

ID=83334968

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210867137.1A Pending CN115109810A (en) 2022-07-22 2022-07-22 Fructo-oligosaccharide and preparation method thereof

Country Status (1)

Country Link
CN (1) CN115109810A (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4317880A (en) * 1980-06-03 1982-03-02 Cpc International Inc. Process for the production of fructose polymers and high fructose syrups
US5998177A (en) * 1998-11-19 1999-12-07 Neose Technologies, Inc. Process for processing sucrose into glucose
CN1335402A (en) * 2001-08-12 2002-02-13 广西大学 Production process of cane-fruit oligosaccharide with immobilized fructose-base transferase
CN101313074A (en) * 2005-11-22 2008-11-26 金克克国际有限公司 In situ fructooligosaccharide production and sucrose reduction
CN104480166A (en) * 2014-12-04 2015-04-01 山东百龙创园生物科技有限公司 Production of fructo-oligosaccharide by virtue of amylase method
CN110331176A (en) * 2019-06-19 2019-10-15 安徽民祯生物工程有限公司 A method of oligofructose being made by raw material of raw sugar
WO2023173705A1 (en) * 2022-03-16 2023-09-21 桂林莱茵生物科技股份有限公司 Sweetening agent composition, preparation method therefor and use thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4317880A (en) * 1980-06-03 1982-03-02 Cpc International Inc. Process for the production of fructose polymers and high fructose syrups
US5998177A (en) * 1998-11-19 1999-12-07 Neose Technologies, Inc. Process for processing sucrose into glucose
CN1335402A (en) * 2001-08-12 2002-02-13 广西大学 Production process of cane-fruit oligosaccharide with immobilized fructose-base transferase
CN101313074A (en) * 2005-11-22 2008-11-26 金克克国际有限公司 In situ fructooligosaccharide production and sucrose reduction
US20100040728A1 (en) * 2005-11-22 2010-02-18 Genencor International, Inc. Situ Fructooligosaccharide Production and Sucrose Reduction
CN104480166A (en) * 2014-12-04 2015-04-01 山东百龙创园生物科技有限公司 Production of fructo-oligosaccharide by virtue of amylase method
CN110331176A (en) * 2019-06-19 2019-10-15 安徽民祯生物工程有限公司 A method of oligofructose being made by raw material of raw sugar
WO2023173705A1 (en) * 2022-03-16 2023-09-21 桂林莱茵生物科技股份有限公司 Sweetening agent composition, preparation method therefor and use thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
毛多斌;王雪;: "果糖基转移酶及低聚果糖生产研究进展", 广东化工, no. 04, 25 April 2009 (2009-04-25), pages 100 - 103 *
阳元娥, 罗发兴: "低聚果糖制备的研究进展", 郑州轻工业学院学报(自然科学版), no. 04, 30 December 2002 (2002-12-30), pages 74 - 77 *

Similar Documents

Publication Publication Date Title
Crittenden et al. Production, properties and applications of food-grade oligosaccharides
Crittenden et al. Purification of food-grade oligosaccharides using immobilised cells of Zymomonas mobilis
WO2009113652A1 (en) Branched dextrin, process for production thereof, and food or beverage
JP2001520525A (en) Method for processing sucrose into glucose and fructose
CN108410925B (en) Method for preparing resistant dextrin by using compound enzyme
US20050181486A1 (en) Method for the removal of monosaccharide in oligosaccharides production
KR101969040B1 (en) Composition comprising isomalto-oligosaccharide and manufacturing method thereof
CN108949713B (en) Preparation method of aspergillus oryzae fermentation broth and application of aspergillus oryzae fermentation broth in production of fructo-oligosaccharide
WO2010023742A1 (en) Method of producing cariostatic composition
Ibrahim Technological aspects of fructo-oligosaccharides (FOS), production processes, physiological properties, applications and health benefits
JP2003183303A (en) Acidic xylooligosaccharide composition and its manufacturing method
CN115109810A (en) Fructo-oligosaccharide and preparation method thereof
KR101105391B1 (en) Food composition comprising enzymatic hydrolysates of kudzu root and preparation method thereof
EP0607264B1 (en) Increased cyclodextrin production
CN112111542B (en) Preparation method of high-purity isomaltooligosaccharide co-produced resistant dextrin
Hirayama et al. Production and utilization of microbial fructans
JP2003048901A (en) Long-chain xylooligosaccharide composition and method for producing the same
CN106755197B (en) Method for preparing linear maltohexaose by using linear maltooligosaccharide generating enzyme
CN110747245B (en) Method for preparing malt oligosaccharide syrup by using complex enzyme
Lee et al. Glucooligosaccharide production by Leuconostoc mesenteroides fermentation with efficient pH control, using a calcium hydroxide-sucrose solution
KR20220118825A (en) Manufacturing method of isomaltooligosaccharide composition with high dietary fiber content
Grizard et al. Enzymatic synthesis and structure determination of NEO‐FOS
KR101964115B1 (en) Method for producing oligosaccharide-rich molasses, oligosaccharide-rich molasses produced by the same and use thereof
JPH0475747B2 (en)
CN108728504B (en) Fructooligosaccharide composition and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination