阅读说明：本技术 一种难消化保湿糖浆及其制备方法与应用 (Indigestible moisture-retaining syrup and preparation method and application thereof ) 是由 刘双双 张明站 张兴晶 王秀芬 禚商志 聂雯 刘国清 李高聪 梁璐 马婷婷 王学 于 2020-12-15 设计创作，主要内容包括：本发明涉及一种难消化保湿糖浆及其制备方法与应用。所述的难消化保湿糖浆以高麦芽糖浆为原料,先通过普鲁兰酶脱支,再经糖化酶作用后所制备的保湿糖浆,其中麦芽糖的含量为5～10％、难消化低聚糖的总含量为90～95％,葡萄糖+大分子糖的含量小于等于1％。本发明中难消化保湿糖浆的制备方法是以高麦芽糖浆为原料,采用普鲁兰酶与糖化酶复配,经普鲁兰酶作用,将小分子的麦芽糖之间进行缩合反应,形成带分枝的聚合度为DP3-DP6难消化低聚糖,再经糖化酶作用降解其中的可消化成分,并经脱色、离交、浓缩,得到料液,经色谱分离去除单糖和双糖,获得纯度较高的难消化低聚糖,简化了生产工艺,提高了生产效率。(The invention relates to indigestible moisture-retaining syrup and a preparation method and application thereof. The indigestible moisture-keeping syrup is prepared by taking high maltose syrup as a raw material, debranching the high maltose syrup by pullulanase, and then performing the action of saccharifying enzyme, wherein the content of maltose is 5-10%, the total content of indigestible oligosaccharides is 90-95%, and the content of glucose and macromolecular sugar is less than or equal to 1%. The preparation method of the indigestible moisture-keeping syrup adopts high maltose syrup as a raw material, pullulanase and saccharifying enzyme are compounded, small molecular maltose is subjected to condensation reaction under the action of the pullulanase to form indigestible oligosaccharide with a branched polymerization degree of DP3-DP6, digestible components in the indigestible oligosaccharide are degraded under the action of the saccharifying enzyme, feed liquid is obtained through decolorization, ion exchange and concentration, monosaccharide and disaccharide are removed through chromatographic separation, and the indigestible oligosaccharide with high purity is obtained, so that the production process is simplified, and the production efficiency is improved.)

1. The indigestible moisture-keeping syrup is characterized in that high maltose syrup is used as a raw material, debranching is performed through pullulanase, and then the high maltose syrup is subjected to diastase, so that the moisture-keeping syrup is prepared, wherein the maltose content is 5-10%, the total content of indigestible oligosaccharides is 90-95%, and the content of glucose and macromolecular sugar is less than or equal to 1%.

2. A preparation method of indigestible moisture-keeping syrup comprises the following steps:

(1) adjusting the pH value of the high maltose syrup to 5-6, adding pullulanase, reacting for 20-26 h at 50-70 ℃, adding saccharifying enzyme, and continuing to react for 8-16 h at 50-60 ℃ to obtain rough moisturizing syrup;

(2) and (2) adding secondary reverse osmosis water into the rough moisturizing syrup prepared in the step (1), heating to 50-70 ℃ for carrying out first resin separation, then adding powdered activated carbon, decoloring for 25-35 min, filtering, carrying out second resin separation, and then carrying out evaporation concentration under the conditions that the vacuum degree is 0.06-0.09 MPa and the temperature is 50-85 ℃ to obtain the indigestible moisturizing syrup.

3. The preparation method of the indigestible moisture-retaining syrup according to claim 2, wherein in the step (1), the substrate concentration of the high maltose syrup in the step (1) is 60-80%, and the maltose content is not less than 70%.

4. The method for preparing the indigestible moisture-retaining syrup according to claim 2, wherein the pullulanase is added in the step (1) in an amount of 1L-2L/T.DS, and the enzyme activity is 3000 μ/mL; the addition amount of the saccharifying enzyme is 0.5L-1L/T.DS, and the enzyme activity is 110000 mu/mL.

5. The preparation method of the indigestible moisture-retaining syrup according to claim 2, wherein the glucose content in the crude moisture-retaining syrup in the step (1) is 40-45%, the maltose content is 25-30%, the total content of indigestible oligosaccharides is 25-30%, and the content of macromolecular sugars is 1-2%.

6. The preparation method of the indigestible moisture-retaining syrup according to claim 2, wherein the mass ratio of the secondary reverse osmosis water to the crude moisture-retaining syrup in the step (2) is (2-3): (1-2).

7. The method for preparing indigestible moisture-retaining syrup according to claim 2, wherein in the first resin separation process in the step (2), calcium type cation resin is used as separation resin, and secondary reverse osmosis water is used as eluent; the adding amount of the activated carbon is 0.5-1.5% of the mass of the rough moisturizing syrup.

8. The preparation method of the indigestible moisture-retaining syrup according to claim 2, wherein in the second resin separation process in the step (2), strong acid cation resin is used as a cation column, weak base anion resin is used as an anion column, the flow rate is 3 times of the resin volume per hour, and the strong acid cation resin, the weak base anion resin and the weak base anion resin sequentially pass through the cation column, the anion column and the cation column at 35-55 ℃.

9. The method for preparing indigestible moisture retaining syrup according to claim 2, wherein the concentration in the step (2) is performed until the solid content of the syrup is 75% or more.

10. The indigestible moisture retaining syrup according to claim 1, which is used in the fields of food, medicine, health products and daily chemical products.

Technical Field

The invention belongs to the technical field of moisturizing, and particularly relates to indigestible moisturizing syrup and a preparation method and application thereof.

Background

In foods (such as caramel treats, cakes and bread), medical and sanitary products and daily chemical products, the quality of the effect of the selected humectant has important influence on the quality of the products, and particularly the effect of the humectant in the foods directly influences the shelf life, the mouthfeel and the quality guarantee period of the products. The humectant is a moisture retention agent of the product and has an important effect on keeping the stability of a product system. At present, the most commonly used natural moisturizing agents such as Hyaluronic Acid (HA) and amino acid moisturizing agents such as methylglycine proline have good moisturizing effect, but the sources of the natural moisturizing agents are relatively lacking, so that the application range of the natural moisturizing agents is limited; the conventional chemical synthesized humectant such as glycerin has a general moisture retention property and a remarkable moisture absorption property, and the moisture retention effect is changed due to the change of the environment. The main component of the food humectant on the market is malto-oligosaccharide, which can prevent water from evaporating easily, has good effects on moisturizing various foods and maintaining the quality of the foods, and can inhibit the formation of crystals of sucrose and glucose. Starch-based foods such as breads and desserts are often hardened upon storage, and the addition of isomaltooligosaccharides prevents starch retrogradation and prolongs the shelf life of the food.

The production process of malto-oligosaccharide mainly uses starch or starchiness as raw material, and adopts the action of high-temperature-resistant enzyme, fungal enzyme or beta-enzyme and transglycosidase to prepare the malto-oligosaccharide. Chinese patent document CN109549059A discloses a moisturizing syrup and a preparation method and application thereof, belonging to the technical field of moisturizing. The invention relates to a moisturizing syrup prepared by taking starch milk as a raw material and performing liquefaction, maltotriose enzyme and beta-amylase saccharification, enzyme deactivation and pullulanase and maltotetraose enzyme saccharification, wherein maltose is 15-25%, maltotriose is 35-45%, maltotetraose is 30-40%, and glucose and macromolecular sugar are less than or equal to 10%. The disadvantages of the syrup are that the prepared moisturizing and antiseptic effects of the moisturizing syrup are still insufficient, and the syrup does not have the characteristic that isomaltooligosaccharide is not easy to digest, and cannot be suitable for special people.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides indigestible moisture-retaining syrup and a preparation method and application thereof. The moisture-keeping syrup has the functional characteristics of isomaltooligosaccharide, low sweetness and osmotic pressure, can obviously proliferate intestinal probiotics, and does not cause diarrhea.

The technical scheme of the invention is as follows:

the indigestible moisture-keeping syrup is characterized in that high maltose syrup is used as a raw material, debranching is performed through pullulanase, and then the high maltose syrup is subjected to diastase, so that the moisture-keeping syrup is prepared, wherein the maltose content is 5-10%, the total content of indigestible oligosaccharides is 90-95%, and the content of glucose and macromolecular sugar is less than or equal to 1%.

The indigestible oligosaccharide is an oligosaccharide with the polymerization degree of DP3-DP 6; the macromolecular sugar is a biological substance with the relative molecular weight of more than 5000.

The invention also provides a preparation method of the indigestible moisture-keeping syrup, which comprises the following steps:

(1) adjusting the pH value of the high maltose syrup to 5-6, adding pullulanase, reacting for 20-26 h at 50-70 ℃, adding saccharifying enzyme, and continuing to react for 8-16 h at 50-60 ℃ to obtain rough moisturizing syrup;

(2) and (2) adding secondary reverse osmosis water into the rough moisturizing syrup prepared in the step (1), heating to 50-70 ℃ for carrying out first resin separation, then adding powdered activated carbon, decoloring for 25-35 min, filtering, carrying out second resin separation, and then carrying out evaporation concentration under the conditions that the vacuum degree is 0.06-0.09 MPa and the temperature is 50-85 ℃ to obtain the indigestible moisturizing syrup.

According to the invention, the substrate concentration of the high maltose syrup in the step (1) is preferably 60-80%, and the content of maltose is more than or equal to 70%.

According to the invention, the addition amount of the pullulanase in the step (1) is 1L-2L/T.DS, and the enzyme activity is 3000 mu/mL.

According to the invention, the addition amount of the saccharifying enzyme in the step (1) is 0.5L-1L/T.DS, and the enzyme activity is 110000 mu/mL.

According to the invention, preferably, in the rough moisturizing syrup in the step (1), the content of glucose is 40-45%, the content of maltose is 25-30%, the total content of indigestible oligosaccharide is 25-30%, and the content of macromolecular sugar is 1-2%.

According to the invention, the mass ratio of the secondary reverse osmosis water to the crude moisturizing syrup in the step (2) is (2-3): (1-2).

According to the invention, in the first resin separation process in the step (2), calcium type cation resin is used as the separation resin, and secondary reverse osmosis water is used as the eluent.

According to the invention, the adding amount of the activated carbon in the step (2) is preferably 0.5-1.5% of the mass of the crude moisturizing syrup.

According to the invention, in the second resin separation process in the step (2), strong acid cation resin is used as an anode column, weak base anion resin is used as an cathode column, the flow rate is 3 times of the resin volume per hour, and the strong acid cation resin, the weak base anion resin and the weak base anion resin are sequentially subjected to the anode column-cathode column-anode column at the temperature of 35-55 ℃.

Preferably, according to the invention, the concentration in step (2) means concentration until the solid content of the syrup is 75% or more.

The indigestible moisture-retaining syrup disclosed by the invention is applied to the fields of food, medicines, health-care products, daily chemical products and the like.

The invention has the beneficial effects that:

1. the preparation method of the indigestible moisture-keeping syrup adopts high maltose syrup as a raw material, pullulanase and saccharifying enzyme are compounded, small molecular maltose is subjected to condensation reaction under the action of the pullulanase to form indigestible oligosaccharide with a branched polymerization degree of DP3-DP6, digestible components in the indigestible oligosaccharide are degraded under the action of the saccharifying enzyme, feed liquid is obtained through decolorization, ion exchange and concentration, monosaccharide and disaccharide are removed through chromatographic separation, and the indigestible oligosaccharide with high purity is obtained, so that the production process is simplified, and the production efficiency is improved.

2. The indigestible moisture-keeping syrup provided by the invention has the functional characteristics of low isomaltose hypgather sweetness and low osmotic pressure, can obviously proliferate intestinal probiotics, does not cause side effects such as diarrhea and the like, can meet the requirement of people on sweetness, and is more suitable for being eaten by obese people, patients with diabetes, cardiovascular diseases and gastrointestinal diseases and producing functional food.

3. The indigestible moisture-preserving syrup prepared by the invention has better moisture-preserving and corrosion-preventing effects, the moisture-preserving rate reaches over 155 in 48 hours under the conditions of 25 ℃ and 40% of relative humidity, and the mildew time is over 220 hours when cakes are added with the moisture-preserving syrup under the conditions of no package, 20 ℃ and 50-60% of environmental humidity.

Detailed Description

The present invention will be further described by way of examples, which are not intended to limit the scope of the present invention. It will be understood by those skilled in the art that the equivalent substitutions and modifications made in the present disclosure are within the scope of the present invention.

The materials and the medicines involved in the invention are common commercial products, the enzymatic activity of the pullulanase is 3000 mu/mL, and the enzymatic activity of the saccharifying enzyme is 110000 mu/mL.

Example 1

A preparation method of indigestible moisture-keeping syrup comprises the following steps:

(1) adjusting the pH value of malt syrup (the content of the malt syrup is 70%) with the substrate concentration of 80% to 5.3, adding 1L/T.DS pullulanase, reacting at 60 ℃ for 24 hours, adding saccharifying enzyme, and continuing to react at 60 ℃ for 12 hours;

(2) adding secondary reverse osmosis water into the coarse moisturizing syrup prepared in the step (1), heating to 60 ℃, then using calcium type cation resin as separation resin, using the secondary reverse osmosis water as eluent to carry out column passing, then adding 1% powdered activated carbon, uniformly stirring, decoloring for 30min, then adopting a plate-and-frame filter press to filter the activated carbon, using strong acid cation resin as a positive column and weak base anion resin as a negative column, wherein the flow rate is 3 times of the volume of the resin per hour, carrying out secondary resin separation by sequentially passing through the positive column, the negative column and the positive column at 40 ℃, and then carrying out evaporation concentration under the conditions that the vacuum degree is 0.06MPa and the temperature is 60 ℃ to obtain the hardly digestible moisturizing syrup.

In the rough moisturizing syrup in the step (1), the glucose content is 43.5 percent, the maltose content is 28.7 percent, the total content of indigestible oligosaccharide is 26.5 percent, and the content of macromolecular sugar is 1.8 percent

The indigestible moisture-keeping syrup prepared in this example has a glucose content of 0.8%, a maltose content of 7.3%, and a total indigestible oligosaccharide content of 91.9%.

Example 2

A preparation method of indigestible moisture-keeping syrup comprises the following steps:

(1) adjusting the pH value of malt syrup (the content of malt syrup is 75%) with the concentration of a substrate of 70% to 5, adding 2L/T.DS pullulanase, reacting at 50 ℃ for 26h, adding saccharifying enzyme, and continuously reacting at 60 ℃ for 16h to obtain crude moisturizing syrup;

(2) adding secondary reverse osmosis water into the coarse moisturizing syrup prepared in the step (1), heating to 50 ℃, then using calcium type cation resin as separation resin, using the secondary reverse osmosis water as eluent to carry out column passing, then adding 1% powdered activated carbon, uniformly stirring, decoloring for 25min, then adopting a plate-and-frame filter press to filter the activated carbon, using strong acid cation resin as a positive column and weak base anion resin as a negative column, wherein the flow rate is 3 times of the volume of the resin per hour, carrying out secondary resin separation by sequentially passing through the positive column, the negative column and the positive column at 40 ℃, and then carrying out evaporation concentration under the conditions that the vacuum degree is 0.08MPa and the temperature is 50 ℃ to obtain the hardly digestible moisturizing syrup.

In the rough moisturizing syrup in the step (1), the glucose content is 35.2%, the maltose content is 45.3%, the total content of indigestible oligosaccharide is 13.8%, and the content of macromolecular sugar is 5.7%

The indigestible moisture-retaining syrup prepared in this example had a maltose content of 8.2% and a total indigestible oligosaccharide content of 91.8%.

Example 3

A preparation method of indigestible moisture-keeping syrup comprises the following steps:

(1) adjusting the pH value of malt syrup (the content of malt syrup is 80%) with the concentration of a substrate of 80% to 6, adding 2L/T.DS pullulanase, reacting at 70 ℃ for 20h, adding saccharifying enzyme, and continuously reacting at 60 ℃ for 16h to obtain crude moisturizing syrup;

(2) adding secondary reverse osmosis water into the coarse moisturizing syrup prepared in the step (1), heating to 70 ℃, then using calcium type cation resin as separation resin, using the secondary reverse osmosis water as eluent to carry out column passing, then adding 1% powdered activated carbon, uniformly stirring, decoloring for 35min, then adopting a plate-and-frame filter press to filter the activated carbon, using strong acid cation resin as a positive column and weak base anion resin as a negative column, wherein the flow rate is 3 times of the volume of the resin per hour, carrying out secondary resin separation by sequentially passing through the positive column, the negative column and the positive column at 40 ℃, and then carrying out evaporation concentration under the conditions that the vacuum degree is 0.09MPa and the temperature is 85 ℃ to obtain the hardly digestible moisturizing syrup.

In the crude moisturizing syrup in the step (1), the glucose content is 41.8%, the maltose content is 33.2%, and the total content of indigestible oligosaccharide is 20.87%

The indigestible moisture-retaining syrup prepared in this example had a maltose content of 5.4% and a total indigestible oligosaccharide content of 94.6%.

Comparative example 1

The moisturizing syrup is prepared according to Chinese patent document CN 109549059A.

In the moisturizing syrup prepared by the comparative example, maltose is 20%, maltotriose is 40%, maltotetraose is 35%, and glucose + macromolecular sugar is 5%.

Comparative example 2

The moisturizing syrup is produced according to the traditional process.

The moisture-keeping syrup prepared by the comparative example contains 37.8% of maltose, 37.6% of maltotriose, 9.8% of maltotetraose and 10.8% of glucose.

Comparative example 3

Changing the experimental raw materials, adjusting the pH value of malt syrup (the content of the malt syrup is 50%) with the substrate concentration of 80% to 5.3 under the same other conditions as in example 1, adding 1L/T.DS pullulanase, reacting at 60 ℃ for 24 hours, adding saccharifying enzyme, and continuing to react at 60 ℃ for 12 hours; the glucose content in the crude moisture-keeping syrup is 70.5%, the maltose content is 23.4%, the total content of indigestible oligosaccharide is 3.5%, and the macromolecule content is 2.5%.

Test example 1

The sweetness of the sucrose is 100 by taking the sweetness of the sucrose as a standard

The sweetness detection method comprises the following steps: the sweetness detection method specified in GB 8270-.

TABLE 1

Product(s)	Sweetness level
		Sucrose	100
Example 1	23.8
		Example 2	24.6
Example 3	25.2
		Comparative example 1	26.8
Comparative example 2	36.1
		Comparative example 3	52.6

Test example 2

The moisturizing effect of the different moisturizing syrups is shown in table 2 below:

table 2: moisture retention rate (25 ℃, relative humidity 40%) for 48h

Product(s)	Moisture retention rate
		Example 1	172
Example 2	161
		Example 3	157
Comparative example 1	118
		Comparative example 2	134
Comparative example 3	92

Test example 3

Experiment of antiseptic effect of different moisturizing syrups:

the moisturizing syrups prepared in examples 1 to 3 and comparative examples 1 to 3 were added to the cake at a ratio of 10% (by weight), the other ingredients and the preparation method of the cake were completely consistent, and the molding time of different cakes was observed under the conditions of no package, 20 ℃ and 50 to 60% of ambient humidity, and the results are shown in table 3 below:

product(s)	Mildew time (h)
		Example 1	243
Example 2	231
		Example 3	224
Comparative example 1	212
		Comparative example 2	176
Comparative example 3	124

It can be seen from the above comparative experiments that the moisturizing syrups obtained in examples 1 to 3 of the present invention, especially example 1, are superior to those obtained in comparative examples 1 and 2 in terms of moisturizing performance and preservative performance, and have lower sweetness, and are softer and purer.