Anti-digestion distarch phosphate and preparation method thereof

Abstract

The invention provides anti-digestion distarch phosphate and a preparation method thereof, and belongs to the field of food additives. The method comprises the following steps: (1) mixing starch with water to obtain a starch emulsion, and then carrying out gelatinization reaction to obtain starch gelatinized liquid; (2) adding sodium salt and a cross-linking agent into the starch gelatinization liquid, uniformly stirring, adjusting the pH value to be alkaline, and then carrying out esterification cross-linking reaction to obtain distarch phosphate crude liquid; and (3) sequentially carrying out pH regulation, leaching, separation, drying and crushing on the distarch phosphate crude liquid to obtain distarch phosphate. According to the anti-digestion distarch phosphate obtained in the invention, the dietary fiber content is greater than or equal to 95%, the drying loss is less than or equal to 8%, the phosphorus content is less than or equal to 0.05%, the pH value is 5.5-7.5, and the anti-digestion distarch phosphate has the effects of resisting digestion and supplementing dietary fibers; the distarch phosphate preparation process adopted by the invention has the characteristics that the esterification efficiency is improved, the dosage of the cross-linking agent is reduced, the water consumption is low, and the pollution discharge is less.

Description

Technical Field

[0001] The invention relates to the field of food additives, and in particular to a digestion-resistant distarch phosphate and a preparation method thereof. Background Art

[0002] Distarch phosphate has the advantages of stable viscosity, good fluidity, elasticity, easy twisting, and strong wear resistance, and is usually used as a thickener, emulsifier, stabilizer, gelling agent, etc. Its dietary fiber content is low or almost non-existent, and generally does not have the function of supplementing dietary fiber.

[0003] Chinese patent CN109678978A discloses a preparation process of distarch phosphate, wherein the starch is ultrasonically treated with an activator, and then refrigerated and subjected to micro-irradiation, followed by centrifugation, ultrasonic washing, and drying to obtain the distarch phosphate. The disclosed preparation process belongs to dry preparation, and the distarch phosphate prepared by the method has the disadvantages of low product quality and low cross-linking agent utilization. Chinese patent CN118580381A discloses a production method of oxidized modified starch based on composite processing, wherein the starch raw material is oxidized and modified with sodium hypochlorite, and the oxidized modified starch is obtained by filtering, washing, drying, and crushing. The preparation process disclosed in the patent has a large water consumption, a large sewage discharge pressure, and a relatively high reagent use cost. Chinese patent CN102086233B discloses a modified starch and a production method using cassava as raw material, wherein cassava is used as raw material, succinic anhydride is added after activation treatment, and then washed, dehydrated, dried, crushed, and sieved to obtain the cassava modified starch. The succinic anhydride used in the preparation process has a pungent odor and has certain irritation and corrosion effects on the eyes, skin and respiratory tract. At the same time, it is found that succinic anhydride is more widely used in coatings, pesticides, fuels, etc., which has certain safety risks. The phosphate distarch obtained by the process described in the above Chinese patents is not resistant to digestion, and there are problems such as low esterification efficiency and low cross-linking agent utilization in the preparation process. Summary of the invention

[0004] In view of this, the object of the present invention is to provide a digestibility-resistant distarch phosphate and a preparation method thereof; the digestibility-resistant distarch phosphate obtained in the present invention has a dietary fiber content of ≥95%, a drying loss of ≤8%, a phosphorus content of ≤0.05%, a pH of 5.5-7.5, and has the effects of digestion resistance and dietary fiber supplementation; the preparation process of distarch phosphate adopted in the present invention has the characteristics of improved esterification efficiency, reduced cross-linking agent dosage, low water consumption, and less sewage discharge.

[0005] In a first aspect, the present invention provides a method for preparing digestion-resistant distarch phosphate, comprising the following steps:

[0006] Step (1) mixing starch and water to obtain starch emulsion, and then performing gelatinization reaction to obtain starch gelatinized liquid;

[0007] Step (2) adding sodium salt and a cross-linking agent to the starch gelatinized liquid, stirring evenly, adjusting the pH value to alkaline, and then performing an esterification and cross-linking reaction to obtain a crude distarch phosphate solution;

[0008] Step (3) sequentially adjusts the pH value of the crude distarch phosphate solution, rinses, separates, dries, and crushes the crude distarch phosphate solution to obtain the distarch phosphate solution.

[0009] Preferably, the solid content of the starch emulsion in step (1) is 40-55%.

[0010] Preferably, the gelatinization reaction temperature in step (1) is 60-70°C, the pH value is 4.5-6.5, the stirring speed is 30-60 rpm, and the reaction time is 40-60 min.

[0011] Preferably, the mass ratio of starch dry basis to sodium salt and cross-linking agent in the starch gelatinized liquid in step (2) is 100:(3-6):(5-10). By adopting the above technical scheme, the exposure probability and quantity of glucose hydroxyl groups in starch are greatly increased through gelatinization reaction, so that the contact probability of glucose hydroxyl groups with phosphate is increased, thereby more efficiently carrying out the replacement reaction, improving the esterification efficiency, cross-linking agent utilization rate, reducing the amount of cross-linking agent and water consumption, and reducing sewage discharge.

[0012] Preferably, the cross-linking agent is sodium trimetaphosphate.

[0013] Preferably, the stirring speed in step (2) is 50-80 rpm.

[0014] Preferably, in step (2), the pH value is adjusted to 11-12; the regulator used to adjust the pH is 1 mol / L NaOH solution.

[0015] Preferably, the temperature of the esterification cross-linking reaction in step (2) is 40-50° C., and the reaction time is 4-8 hours.

[0016] Preferably, the pH in step (3) is adjusted to 5.5-6.5

[0017] In a second aspect, the present invention provides a digestibility-resistant distarch phosphate prepared by the above-mentioned preparation method.

[0018] Beneficial technical effects:

[0019] 1. The digestibility-resistant distarch phosphate involved in the present invention has the characteristics of dietary fiber content ≥95%, drying loss ≤8%, phosphorus content ≤0.05%, and pH 5.5-7.5. All indicators are better than national standard requirements and conventional products. It can be used to supplement the dietary fiber content in daily diet, expanding the use scenarios and scope of distarch phosphate.

[0020] 2. The present invention improves the esterification efficiency and the utilization rate of the cross-linking agent and reduces the amount of the cross-linking agent used. The esterification efficiency is improved and the utilization rate of the cross-linking agent is improved. The amount of the cross-linking agent used is low and the residual amount of the cross-linking agent is low. Therefore, the elution process uses less water, which reduces the difficulty of industrial production. DETAILED DESCRIPTION

[0021] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as limiting the present invention, but should be understood as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0022] It should be understood that the terms described in the present invention are only for describing special embodiments and are not intended to limit the present invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper and lower limits of the scope is also specifically disclosed. Each smaller range between the intermediate value in any stated value or stated range and any other stated value or intermediate value in the described range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the scope.

[0023] Unless otherwise indicated, all technical and scientific terms used herein have the same meanings as those generally understood by those skilled in the art. Although the present invention describes only preferred methods and materials, any methods and materials similar or equivalent to those described herein may also be used in the implementation or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and / or materials associated with the documents. In the event of a conflict with any incorporated document, the content of this specification shall prevail.

[0024] It will be apparent to those skilled in the art that various modifications and variations may be made to the specific embodiments of the present invention description without departing from the scope or spirit of the present invention. Other embodiments derived from the present invention description will be apparent to those skilled in the art. The present application description and examples are exemplary only.

[0025] The words “include,” “including,” “have,” “contain,” etc. used in this document are open-ended terms, meaning including but not limited to.

[0026] The "room temperature" and "normal temperature" mentioned in the present invention are all calculated as 25±2°C unless otherwise specified.

[0027] The raw materials used in the following examples of the present invention are commercially available unless otherwise specified.

[0028] The detection items of the present invention are:

[0029] The preparation process of digestibility-resistant distarch phosphate mainly includes the following three parts: the first part is the index requirements of distarch phosphate involved in the Chinese national standard GB29926-2013; the second part is the comparison of the usage of sodium salt and cross-linking agent in the preparation process; the third part is the dietary fiber content of the digestibility-resistant distarch phosphate obtained; the fourth part is the detection of the phosphorus content, drying loss, phosphorus content in the elution liquid of the finished product obtained according to the preparation process involved in the present invention, and the comparison of water consumption when the sewage discharge standard is reached.

[0030] Example 1

[0031] This embodiment provides a method for preparing digestion-resistant distarch phosphate, the steps are as follows:

[0032] (1) Starch was used as a raw material, and purified water was added to adjust the starch emulsion to have a solid content of 40%. The pH value of the starch emulsion was then adjusted to 5, and a gelatinization reaction was performed at a stirring speed of 50 rpm and 65° C. for 50 min to obtain a starch gelatinized liquid.

[0033] (2) To the starch gelatinized liquid, add 4% sodium chloride and 8% sodium trimetaphosphate in a dry basis of starch in sequence, and stir evenly at 60 rpm; then use 1 mol / L NaOH solution to adjust the pH value of the starch milk to 11.5; then place it in a 45°C water bath and perform esterification and cross-linking reaction for 4 hours to obtain a crude distarch phosphate solution.

[0034] (3) The pH value of the crude distarch phosphate solution was adjusted to 5.8 using 1 mol / L HCl solution. The crude starch was then washed and separated using a centrifuge, and the resulting wet starch was dried using a drum dryer. The amount of water used in the washing step was recorded, and the phosphorus content of the washing solution was tested.

[0035] After drying, the phosphate distarch is obtained, and its dietary fiber content, phosphorus content, drying loss and pH value are tested according to the national standard method.

[0036] The digestibility-resistant distarch phosphate obtained in Example 1 had a dietary fiber content of 96.51%, a phosphorus content of 0.03%, a drying loss of 6.13%, a pH value of 5.8, a leaching water volume of 3.75 L / kg, and a phosphorus content of 4.23 mg / L in the leaching liquid.

[0037] Example 2

[0038] This embodiment provides a method for preparing digestion-resistant distarch phosphate, the steps are as follows:

[0039] (1) Starch was used as a raw material, and purified water was added to adjust the starch milk to have a solid content of 45%. The pH value was then adjusted to 5.5, and a gelatinization reaction was carried out at a stirring speed of 60 rpm and 70°C for 60 min to obtain a starch gelatinized liquid.

[0040] (2) To the starch gelatinized liquid, add 6% sodium chloride and 10% sodium trimetaphosphate in the amount of starch dry basis, start stirring at 80 rpm, and adjust the pH value of the starch milk to 11.8 using 1 mol / L NaOH solution; then place the mixture in a 45°C water bath and perform esterification and cross-linking reaction for 4 hours to obtain a crude distarch phosphate solution.

[0041] (3) Using 1 mol / L HCl solution, the pH value of the crude distarch phosphate solution was adjusted to 6.2; then, a centrifuge was used for elution and separation, and the obtained wet starch was dried using a drum dryer; the amount of water used in the elution step was recorded, and the elution solution was tested for phosphorus content;

[0042] After drying, the phosphate distarch is obtained, and its dietary fiber content, phosphorus content, drying loss and pH value are tested according to the national standard method.

[0043] The digestibility-resistant distarch phosphate obtained in Example 2 has a dietary fiber content of 96.09%, a phosphorus content of 0.04%, a drying loss of 5.93%, a pH value of 5.9, a leaching water volume of 3.86 L / kg, and a phosphorus content of the leaching liquid of 4.36 mg / L.

[0044] Example 3

[0045] This embodiment provides a method for preparing digestion-resistant distarch phosphate, the steps are as follows:

[0046] (1) Starch was used as a raw material, and purified water was added to adjust the starch milk to a solid content of 55%; then the pH value was adjusted to 4.5, and gelatinization reaction was carried out at a stirring speed of 30 rpm and 60°C for 40 minutes to obtain a starch gelatinized liquid;

[0047] (2) Add 3% sodium chloride and 5% sodium trimetaphosphate to the starch gelatinized solution in turn, start stirring at 50 rpm, and use 1 mol / L NaOH solution to adjust the pH value of the starch milk to 11.3; then place it in a 40°C water bath and perform esterification and cross-linking reaction for 8 hours to obtain a crude distarch phosphate solution.

[0048] (3) Using 1 mol / L HCl solution, the pH value of the crude distarch phosphate solution was adjusted to 5.1; then, a centrifuge was used for elution and separation, and the obtained wet starch was dried using a drum dryer; the amount of water used in the elution step was recorded, and the elution solution was tested for phosphorus content;

[0049] After drying, the phosphate distarch is obtained, and its dietary fiber content, phosphorus content, drying loss and pH value are tested according to the national standard method.

[0050] The digestibility-resistant distarch phosphate obtained in Example 3 had a dietary fiber content of 96.01%, a phosphorus content of 0.03%, a drying loss of 5.97%, a pH value of 5.9, a leaching water volume of 3.91 L / kg, and a phosphorus content of 4.33 mg / L in the leaching liquid.

[0051] Comparative Example 1

[0052] In this comparative example, digestion-resistant distarch phosphate was prepared according to the preparation method of Example 1, except that the gelatinization reaction temperature in step (2) was 55° C. and the reaction time was 70 min.

[0053] The digestibility-resistant distarch phosphate obtained in Comparative Example 1 had a dietary fiber content of 58.40%, a phosphorus content of 0.35%, a drying loss of 12.78%, a pH value of 5.5, a leaching water volume of 3.78 L / kg, and a phosphorus content of 4.19 mg / L in the leaching liquid.

[0054] Comparative Example 2

[0055] In this comparative example, digestion-resistant distarch phosphate was prepared according to the preparation method of Example 1, except that the pH value of the gelatinization reaction conditions in step (2) was 7.0;

[0056] The digestibility-resistant distarch phosphate obtained in Comparative Example 2 had a dietary fiber content of 64.16%, a phosphorus content of 0.39%, a drying loss of 11.93%, a pH value of 6.6, a rinsing water volume of 4.07 L / kg, and a phosphorus content of 4.01 mg / L in the rinsing liquid.

[0057] Comparative Example 3

[0058] In this comparative example, digestion-resistant distarch phosphate was prepared according to the preparation method of Example 1, except that in step (3), the amount of sodium trimetaphosphate added was 4% of the dry weight of starch;

[0059] The digestibility-resistant distarch phosphate obtained in Comparative Example 3 had a dietary fiber content of 67.4%, a phosphorus content of 0.25%, a drying loss of 12.88%, a pH value of 7.2, a leaching water volume of 3.86 L / kg, and a phosphorus content of the leaching liquid of 3.98 mg / L.

[0060] Comparative Example 4

[0061] In this comparative example, digestibility-resistant distarch phosphate was prepared according to the preparation method of Example 1, except that the pH adjuster in step (2) was 1 mol / L NaOH, and the pH value was adjusted to 10.

[0062] The digestibility-resistant distarch phosphate obtained in Comparative Example 4 had a dietary fiber content of 64.22%, a phosphorus content of 0.36%, a drying loss of 10.96%, a pH value of 5.4, a leaching water volume of 3.73 L / kg, and a phosphorus content of 4.22 mg / L in the leaching liquid.

[0063] Comparative Example 5

[0064] In this comparative example, digestion-resistant distarch phosphate was prepared according to the preparation method of Example 1, except that the esterification and cross-linking reaction conditions in step (2) were 3 hours.

[0065] The digestibility-resistant distarch phosphate obtained in Comparative Example 5 had a dietary fiber content of 59.97%, a phosphorus content of 0.38%, a drying loss of 11.03%, a pH value of 5.5, a leaching water volume of 3.80 L / kg, and a phosphorus content of 4.25 mg / L in the leaching liquid.

[0066] Comparative Example 6

[0067] In this comparative example, digestion-resistant distarch phosphate was prepared according to the preparation method of Example 1, except that in step (2), the amount of sodium trimetaphosphate added was 11% of the dry weight of starch;

[0068] The digestibility-resistant distarch phosphate obtained in Comparative Example 6 had a dietary fiber content of 61.86%, a phosphorus content of 0.37%, a drying loss of 10.25%, a pH value of 7.1, a leaching water volume of 121.4 L / kg, and a phosphorus content of 4.11 mg / L in the leaching liquid.

[0069] In summary, the present invention has found in the experimental process that after subjecting starch milk to gelatinization reaction and then to phosphation reaction, the obtained distarch phosphate not only has resistance to digestion, but also has higher esterification efficiency and less cross-linking agent usage during the reaction process; and the above technical effects are obtained by setting the reaction conditions.

[0070] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing digestion-resistant distarch phosphate, characterized in that: The following steps are involved: Step (1) mixing starch and water to obtain starch emulsion, and then performing gelatinization reaction to obtain starch gelatinized liquid; Step (2) adding sodium salt and a cross-linking agent to the starch gelatinized liquid, stirring evenly, adjusting the pH value to alkaline, and then performing an esterification and cross-linking reaction to obtain a crude distarch phosphate solution; Step (3) sequentially adjusting the pH of the crude distarch phosphate solution, eluting, separating, drying, and crushing to obtain distarch phosphate; The solid content of the starch emulsion in step (1) is 40-55%; The gelatinization reaction temperature in step (1) is 60-70°C, the pH value is 4.5-6.5, the stirring speed is 30-60 rpm, and the reaction time is 40-60 min; In the step (2), the mass ratio of the starch dry basis to the sodium salt and the cross-linking agent in the starch gelatinization solution is 100:(3-6):(5-10); The cross-linking agent is sodium trimetaphosphate; In the step (2), the pH value is adjusted to 11-12; the pH regulator used to adjust the pH is 1 mol / L NaOH solution; The temperature of the esterification cross-linking reaction in step (2) is 40-50° C., and the reaction time is 4-8 hours.

2. The preparation method according to claim 1, characterized in that: The stirring speed in step (2) is 50-80 rpm.

3. The preparation method according to claim 1, characterized in that: In the step (3), the pH is adjusted to 5.5-6.

5.

4. A digestion-resistant distarch phosphate, characterized in that: The invention is prepared by the preparation method according to any one of claims 1 to 3.