High-panose material as well as preparation method and application thereof
Through multiple saccharification reactions and retention processes, combined with glucosidase and semi-permeable membrane desalting technology, high-purity high-panose materials were prepared, solving the problems of low panose content and high water activity in isomaltooligosaccharides, thus improving the anti-caries effect of toothpaste.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-24
- Publication Date
- 2026-03-31
AI Technical Summary
In existing technologies, isomaltooligosaccharides have low panose content, wide molecular distribution, high water activity, and are prone to hygroscopicity, thus limiting their effectiveness in products such as toothpaste.
Through multiple saccharification reactions and retention processes, combined with the catalytic characteristics of glucosidase, the reaction conditions were optimized to generate high-purity panose. High-panose material was obtained by desalting with a semi-permeable membrane and resin.
It achieves a panose content of ≥90wt% in high panose materials, with concentrated molecular distribution and reduced water activity, making it suitable for products such as toothpaste and significantly improving the anti-caries effect.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of preparation technology of isomaltooligosaccharides, specifically relating to a high-panol content material, its preparation method, and its application. Background Technology
[0002] Isomaltooligosaccharide (OMOS) is a non-fermentable oligosaccharide composed of glucose linked by α-1,6 glycosidic bonds. Its main components are isomaltooligosaccharide and panose, and it is also known as a bifidobacteria growth promoter. IOS rarely exists in a free state in nature, but as a component of amylopectin or polysaccharides, it is present in small amounts in some fermented foods such as soy sauce, rice wine, or enzymatically processed glucose syrup. It can significantly promote the proliferation of bifidobacteria in the human body, functions as a water-soluble dietary fiber, and has low calorie value and anti-caries properties. Furthermore, the industrial production of IOS uses starch as a raw material and converts it through α-glucosidase. It has a low panose content, with a maximum panose content of only about 20%, a wide component distribution, high water activity, and is easily hygroscopic. Summary of the Invention
[0003] The purpose of this invention is to provide a high-panose material, its preparation method, and its application. The preparation method provided by this invention yields a material with high panose content, concentrated molecular distribution, and low water activity.
[0004] To achieve the above objectives, the present invention provides the following technical solution: This invention provides a method for preparing a high-panose material, comprising the following steps: Maltose syrup is added to glucosidase for the first saccharification reaction. The resulting reaction solution is retained to obtain a first concentrated solution and a first filtrate. The maltose syrup contains ≥80% maltose by mass. The first filtrate and malt syrup are subjected to a second saccharification reaction, and the resulting reaction solution is retained to obtain a second concentrate and a second filtrate. The second filtrate and malt syrup are subjected to a third saccharification reaction, and the resulting reaction solution is retained to obtain a third concentrate and a third filtrate. After combining the first, second, and third concentrates, decolorization and filtration were performed sequentially to obtain the crude liquid. The crude liquid is sequentially desalted, concentrated and dried to obtain a high-panose material; the panose content in the high-panose material is ≥90wt%.
[0005] Preferably, the temperatures of the first saccharification reaction, the second saccharification reaction, and the third saccharification reaction are independently 50~70°C; The holding time for the first saccharification reaction is 6-8 hours, the holding time for the second saccharification reaction is 3-4 hours, and the holding time for the third saccharification reaction is 1-5 hours.
[0006] Preferably, the retention is achieved using a semi-permeable membrane; the pore size of the semi-permeable membrane is 400~500 Da.
[0007] Preferably, the malt syrup contains ≤10% glucose by mass; the malt syrup has a solids content of 35-40 wt% and a pH value of 4.9-5.5.
[0008] Preferably, the mass ratio of the first filtrate to malt syrup is 1:1 to 1:3; and the mass ratio of the second filtrate to malt syrup is 1:3 to 1:6.
[0009] Preferably, the decolorization temperature is 75~85℃, and the holding time is 20~40min.
[0010] Preferably, the flow temperature of the crude liquid during the desalination process is 35~40℃, the flow rate is 1~3 BV / h, and the pH value of the output is 5.0~6.0.
[0011] The present invention also provides a high-panose material prepared by the preparation method described above, wherein the panose content in the high-panose material is ≥90wt%.
[0012] The present invention also provides high-panol material prepared by the preparation method described above, or the application of the high-panol material described above in toothpaste.
[0013] Preferably, the amount of high-panol content material added to the toothpaste is 1-8 wt%.
[0014] The present invention has the following advantages over the prior art: This invention utilizes the catalytic characteristics of glucosidase, selects raw materials with specific compositions, and achieves product-directed processing by controlling the reaction process. When the maltose content in the raw materials is high (≥80%), the reaction preferentially generates panose, while inhibiting the formation of other components such as isomaltose or pantetraose, thereby obtaining high-purity panose, continuously improving the utilization rate of raw materials, and shortening the reaction time.
[0015] Furthermore, the preparation method provided by this invention overcomes the problem of low panose content in traditional isomaltooligosaccharides, successfully preparing high-purity panose and reducing the formation of disaccharides and macromolecular oligosaccharides. Data from the examples show that the product provided by this invention has a panose content ≥90wt% (containing a small amount of maltodextrin), and compared with traditional isomaltooligosaccharides, it has lower water activity and a more concentrated molecular distribution, solving problems such as easy moisture absorption. Detailed Implementation
[0016] This invention provides a method for preparing a high-panose material, comprising the following steps: Maltose syrup was added to glucosidase for the first saccharification reaction, and the resulting reaction solution was retained to obtain the first concentrated solution and the first filtrate. The first filtrate and malt syrup are subjected to a second saccharification reaction, and the resulting reaction solution is retained to obtain a second concentrate and a second filtrate. The second filtrate and malt syrup are subjected to a third saccharification reaction, and the resulting reaction solution is retained to obtain a third concentrate and a third filtrate. After combining the first, second, and third concentrates, decolorization and filtration were performed sequentially to obtain the crude liquid. The crude liquid is sequentially desalted, concentrated and dried to obtain a high-panose material; the panose content in the high-panose material is ≥90wt%.
[0017] In this invention, maltose syrup is added to glucosidase to carry out a first saccharification reaction, and the resulting reaction solution is retained to obtain a first concentrated solution and a first filtrate.
[0018] In one embodiment of the present invention, the maltose syrup contains ≥80% by mass of maltose; the glucose content in the maltose syrup can be ≤10% by mass, specifically ≤8%; the solids content of the maltose syrup can be 35~40wt%, and the pH value can be 4.9~5.5.
[0019] In one embodiment of the present invention, the temperature of the first saccharification reaction can be 50~70℃, specifically 50℃, 55℃, 58℃, 60℃, 65℃ or 70℃; the holding time can be 6~8h, specifically 6h, 7h or 8h. In another embodiment of the present invention, the retention can be achieved using a semi-permeable membrane; the pore size of the semi-permeable membrane can be 400~500 Da.
[0020] After obtaining the first concentrate, the present invention performs a second saccharification reaction on the first filtrate and malt syrup, and retains the resulting reaction solution to obtain the second concentrate and the second filtrate.
[0021] In one embodiment of the present invention, the mass ratio of the first filtrate to maltose syrup can be 1:1 to 1:3, specifically 1:1, 1:2 or 1:3; in another embodiment of the present invention, the temperature of the second saccharification reaction can be 50 to 70°C, specifically 50°C, 55°C, 58°C, 60°C, 65°C or 70°C, and the holding time can be 3 to 4 hours, specifically 3 hours or 4 hours.
[0022] After obtaining the second filtrate, the present invention performs a third saccharification reaction on the second filtrate and malt syrup, and retains the resulting reaction solution to obtain a third concentrate and a third filtrate.
[0023] In one embodiment of the present invention, the mass ratio of the second filtrate to maltose syrup can be 1:3 to 1:6, specifically 1:3, 1:4, 1:5 or 1:6; in another embodiment of the present invention, the temperature of the third saccharification reaction can be 50 to 70°C, specifically 50°C, 55°C, 58°C, 60°C, 65°C or 70°C, and the holding time can be 1 to 5 hours, specifically 2 hours.
[0024] After combining the first, second, and third concentrates, decolorization and filtration were carried out sequentially to obtain the crude liquid.
[0025] In one embodiment of the present invention, the decolorization is preferably performed using activated carbon.
[0026] In one embodiment of the present invention, the decolorization temperature can be 75~85℃, and the holding time can be 20~40min.
[0027] After obtaining the crude liquid, the present invention desalinates, concentrates and dries the crude liquid in sequence to obtain a high-panose material; the high-panose material has a panose content ≥90wt%.
[0028] In one embodiment of the present invention, the desalination is carried out by sequentially using a strong acid cation resin D001 and a weak base anion resin D301P.
[0029] In one embodiment of the present invention, the flow temperature of the crude liquid during the desalination process can be 35~40℃, the flow rate can be 1~3 BV / h, and the pH value of the output can be 5.0~6.0.
[0030] The present invention also provides a high-panose material prepared by the preparation method described in the above technical solution.
[0031] The present invention also provides the application of the high-panose material prepared by the preparation method described above in toothpaste.
[0032] As one embodiment of the present invention, the amount of high-panose material added to the toothpaste can be 1~8wt%, specifically 3~5wt%.
[0033] To further illustrate the present invention, the following detailed description of the embodiments is provided in conjunction with the present invention, but these descriptions should not be construed as limiting the scope of protection of the present invention.
[0034] Example 1 (1) Malt syrup (maltose content in malt syrup is 88wt% and glucose content is 5wt%) was selected as substrate, and the solid content was adjusted to 40% and the pH was 5.4.
[0035] (2) Take the first portion of malt syrup (1000g) and add glucosidase (600mL / T.DS). The reaction is carried out at 58℃. When the reaction is carried out for 8 hours (panose content 35wt%), the reaction is stopped. Then, a semipermeable membrane with a molecular weight cutoff of 500Da is used to retain the reaction solution to obtain concentrated solution (372.8g) and filtrate (627.2g). The concentrated solution is panose 1 (panose content 92%).
[0036] (3) Add the second part of maltose syrup (1254.4g) to the filtrate (627.2g) and continue the second stage reaction (temperature 60℃). After 4 hours, the reaction is stopped (panose content 20.8wt%). Then, a semi-permeable membrane with a molecular weight cutoff of 500Da is used to retain the reaction solution to obtain concentrated solution (419.2g) and filtrate (1462.4g). The concentrated solution is panose 2 (panose content 91.5%).
[0037] (4) Add the third part of maltose syrup (5849.6g) to the filtrate (1462.4g) and continue the third stage reaction (65℃). After 2 hours, the reaction is stopped (panose content 10wt%). Then, a semi-permeable membrane with a molecular weight cutoff of 500Da is used to retain the reaction solution to obtain concentrated solution (791.8g) and filtrate (6520.2g). The concentrated solution is panose 3 (panose content 90.5wt%).
[0038] (5) The three groups of panose concentrates were mixed and decolorized (temperature 80℃, time 30min) and filtered to obtain crude liquid. Then, it was desalted by strong acid cation resin D001 and weak base anion resin D301P (during desalting, the feed temperature was 35℃, the feed speed was 2BV / h, and the output pH was 5.0~6.0). The filtrate was then concentrated by evaporation and dried to prepare high panose material (panose content 91.12%).
[0039] The panose content in Example 1 was determined in accordance with GB / T 23528.4-2025 Oligosaccharide Quality Requirements Part 4: Isomaltooligosaccharides.
[0040] Example 2 (1) Select malt syrup (maltose content in malt syrup is 83wt% and glucose content is 9wt%) as substrate, adjust the solid content to 40% and pH to 5.4 (prepare 3 portions).
[0041] (2) Take the first portion of malt syrup (1000g) and add glucosidase (600mL / T.DS). The reaction is carried out at 58℃. When the reaction has been going on for 7 hours (panose content 30wt%), the reaction solution is then retained by a semipermeable membrane with a molecular weight cutoff of 500Da to obtain a concentrated solution (325.2g) and a filtrate (674.8g). The concentrated solution is panose 1 (panose content 90.4wt%). (3) Add the second part of maltose syrup (2024.4g) to the filtrate (674.8g) and continue the second stage reaction (temperature 60℃). After 4 hours, the reaction was stopped (panose content 17.6wt%). Then, a semi-permeable membrane with a molecular weight cutoff of 500Da was used to retain the reaction solution to obtain concentrated solution (511.6g) and filtrate (2187.6g). The concentrated solution is panose 2 (panose content 91.0%). (4) Add the third part of maltose syrup (10938g) to the filtrate (2187.6g) and continue the third stage reaction (temperature 65℃). After 2 hours, the reaction is stopped (panose content 10wt%). Then, a semi-permeable membrane with a molecular weight cutoff of 500Da is used to retain the reaction solution to obtain concentrated solution (1405.8g) and filtrate (11719.8g). The concentrated solution is panose 3 (panose content 91.5%). (5) The three groups of panose concentrates were mixed and decolorized (temperature 80℃, time 30min) and filtered to obtain crude liquid. Then, it was desalted by strong acid cation resin D001 and weak base anion resin D301P (during desalting, the feed temperature was 35℃, the feed speed was 2BV / h, and the output pH was 5.0~6.0). The filtrate was then concentrated by evaporation and dried to prepare high panose material (panose content 91.22wt%).
[0042] The panose content in Example 2 was determined in accordance with GB / T 23528.4-2025 Oligosaccharide Quality Requirements Part 4: Isomaltooligosaccharides.
[0043] Example 3 (1) Select malt syrup (maltose content in malt syrup is 90wt% and glucose content is 4wt%) as substrate, adjust the solid content to 40% and pH to 5.4 (prepare 3 portions).
[0044] (2) Take the first portion of malt syrup (1000g) and add glucosidase (600mL / T.DS). The reaction is carried out at 58℃. When the reaction has been carried out for 7 hours (panose content 38wt%), the reaction solution is then retained by a semipermeable membrane with a molecular weight cutoff of 500Da to obtain a concentrated solution (403g) and a filtrate (597g). The concentrated solution is panose 1 (panose content 92.4wt%). (3) Add the second part of maltose syrup (597g) to the filtrate (597g) and continue the second stage reaction (temperature 60℃). After 4 hours, the reaction is stopped (panose content 23.5wt%). Then, a semi-permeable membrane with a molecular weight cutoff of 500Da is used to retain the reaction solution to obtain concentrated solution (303.2g) and filtrate (890.8g). The concentrated solution is panose 2 (panose content 90.7%). (4) Add the third part of maltose syrup (2672.4g) to the filtrate (890.8g) and continue the third stage reaction (temperature 65℃). After 2 hours, the reaction is stopped (panose content 15.6wt%). Then, a semi-permeable membrane with a molecular weight cutoff of 500Da is used to retain the reaction solution to obtain concentrated solution (597.3g) and filtrate (2965.9g). The concentrated solution is panose 3 (panose content 91.2%). (5) The three groups of panose concentrates were mixed and decolorized (temperature 80℃, time 30min) and filtered to obtain crude liquid. Then, the crude liquid was desalted by strong acid cation resin D001 and weak base anion resin D301P (during desalting, the feed temperature was 35℃, the feed speed was 2BV / h, and the output pH was 5.0~6.0). The filtrate was then concentrated by evaporation and dried to prepare high panose material (panose content 91.45wt%).
[0045] The panose content in Example 3 was determined in accordance with GB / T 23528.4-2025 Oligosaccharide Quality Requirements Part 4: Isomaltooligosaccharides.
[0046] Comparative Example 1 (1) Select malt syrup (maltose content 70wt% and glucose 4.5wt% in malt syrup) as substrate, adjust solids to 40% and pH to 5.4 (prepare 3 portions).
[0047] (2) Take the first portion of malt syrup (1000g) and add glucosidase (600mL / T.DS). React at 58℃. When the reaction has been going on for 7 hours (panose content 15.6wt%), use a semipermeable membrane with a molecular weight cutoff of 500Da to retain the reaction solution to obtain concentrated solution (211.2g) and filtrate (788.8g). The concentrated solution is panose 1 (panose content 72.4wt%). (3) Add the second part of maltose syrup (2366.4g) to the filtrate (788.8g) and continue the second stage reaction (temperature 60℃). After 4 hours, the reaction is stopped (panose content 11.5wt%). Then, a semi-permeable membrane with a molecular weight cutoff of 500Da is used to retain the reaction solution to obtain concentrated solution (497.3g) and filtrate (2657.9g). The concentrated solution is panose 2 (panose content 71.5%). (4) Add the third part of maltose syrup (13289.5g) to the filtrate (2657.9g) and continue the third stage reaction (temperature 65℃). After 2 hours, the reaction is stopped (panose content 7.3wt%). Then, a semi-permeable membrane with a molecular weight cutoff of 500Da is used to retain the reaction solution to obtain concentrated solution (1613.7g) and filtrate (14333.7g). The concentrated solution is panose 3 (panose content 70.7wt%). (5) The three groups of panose concentrates were mixed and decolorized (temperature 80℃, time 30min) and filtered to obtain crude liquid. Then, the crude liquid was desalted by strong acid cation resin D001 and weak base anion resin D301P (during desalting, the feed temperature was 35℃, the feed speed was 2BV / h, and the output pH was 5.0~6.0). The filtrate was then evaporated, concentrated, and dried to prepare high panose material (panose content 71.03wt%).
[0048] The content of panose in Comparative Example 1 was tested in accordance with GB / T 23528.4-2025 Oligosaccharide Quality Requirements Part 4: Isomaltooligosaccharides.
[0049] Comparative Example 2 (1) Select malt syrup (maltose content in malt syrup is 55wt% and glucose content is 1.2wt%) as substrate, adjust the solid content to 40% and pH to 5.4 (prepare 3 portions).
[0050] (2) Take the first portion of maltose syrup (1000g) and add glucosidase (600mL / T.DS). React at 58℃. When the reaction has been going on for 7 hours (panose content 8.6wt%), use a semipermeable membrane with a molecular weight cutoff of 500Da to retain the reaction solution to obtain concentrated solution (144.3g) and filtrate (855.7g). The concentrated solution is panose 1 (panose content 58.4wt%). (3) Add the second part of maltose syrup (2567.1g) to the filtrate (855.7g) and continue the second stage reaction (temperature 60℃). After 4 hours, the reaction is stopped (panose content 7.2wt%). Then, a semi-permeable membrane with a molecular weight cutoff of 500Da is used to retain the reaction solution to obtain concentrated solution (418.6g) and filtrate (3004.2g). The concentrated solution is panose 2 (panose content 57.7wt%). (4) Add the third part of maltose syrup (15021g) to the filtrate (3004.2g) and continue the third stage reaction (temperature 65℃). After 2 hours, the reaction is stopped (panose content 6.5wt%). Then, a semi-permeable membrane with a molecular weight cutoff of 500Da is used to retain the reaction solution to obtain concentrated solution (1969.5g) and filtrate (16055.7g). The concentrated solution is panose 3 (panose content 58.3%). (5) The three groups of panose concentrates were mixed and decolorized (temperature 80℃, time 30min) and filtered to obtain crude liquid. Then, it was desalted by strong acid cation resin D001 and weak base anion resin D301P (during desalting, the feed temperature was 35℃, the feed speed was 2BV / h, and the output pH was 5.0~6.0). The filtrate was then concentrated by evaporation and dried to prepare high panose material (panose content 58.21wt%).
[0051] The content of panose in Comparative Example 2 was tested in accordance with GB / T 23528.4-2025 Oligosaccharide Quality Requirements Part 4: Isomaltooligosaccharides.
[0052] Comparative Example 3 Traditional isomaltooligosaccharide Using a suitable maltose syrup (55 wt% maltose and 1.2 wt% glucose) as the substrate, the solids content was adjusted to 40% and the pH to 5.4. The reaction was carried out at 60℃. After 24 hours of reaction (15 wt% panose content), the solution was desalted, evaporated and concentrated, and then separated and dried by chromatography to prepare an isomaltooligosaccharide solution (19.5 wt% panose content).
[0053] The content of panose in Comparative Example 3 was determined in accordance with GB / T 23528.4-2025 Oligosaccharide Quality Requirements Part 4: Isomaltooligosaccharides.
[0054] Comparative Example 4 Glucoside transferase (600 mL / T.DS) was added to 1000 g of malt syrup (maltose content 90 wt%, glucose 4 wt%) and the reaction was carried out at 58 °C. The reaction was stopped after 8 h (panose content 19 wt%). Then, a semipermeable membrane with a molecular weight cutoff of 500 Da was used to retain the reaction solution, and a concentrated solution (204.8 g) and a filtrate (795.2 g) were obtained. The concentrated solution was panose (panose content 90.9%).
[0055] The water activity of the high-panose materials obtained in Examples 1-3 and Comparative Examples 1-3 was tested according to the method for determining water activity in GB 5009.238-2016 "Determination of Water Activity in Food". The results are shown in Table 1. The molecular weight of panose in the examples and comparative examples is shown in Table 1.
[0056] Table 1. Water activity test results of high-panose materials obtained in the examples and comparative examples.
[0057] As shown in Table 1, the water activity of the high-panose material prepared by this invention is reduced compared with that of traditional isomaltooligosaccharide.
[0058] The high-panose material or isomaltooligosaccharide solution obtained from the examples and comparative examples was added to toothpaste (Haolai Super White Baking Soda Mint Tea Toothpaste), and antibacterial test was conducted according to the antibacterial experiment in Section 2.1.8 of the "Disinfection Technical Specifications". The test results are shown in Table 2.
[0059] Table 2. Test results of high-panolose materials or isomaltooligosaccharide solutions obtained in the examples and comparative examples.
[0060] As shown in Table 2, the high-panose material provided by this invention, when applied to toothpaste, achieves a removal rate of up to 98% for Streptococcus mutans, greatly enhancing its anti-caries effect in toothpaste.
[0061] Although the above embodiments have provided a detailed description of the present invention, they are only some embodiments of the present invention, and not all embodiments. Other embodiments can be obtained based on these embodiments without creative effort, and these embodiments all fall within the protection scope of the present invention.
Claims
1. A method for preparing a high-panol material, characterized in that, Includes the following steps: Maltose syrup is added to glucosidase for the first saccharification reaction. The resulting reaction solution is retained to obtain a first concentrated solution and a first filtrate. The maltose syrup contains ≥80% maltose by mass. The first filtrate and malt syrup are subjected to a second saccharification reaction, and the resulting reaction solution is retained to obtain a second concentrate and a second filtrate. The second filtrate and malt syrup are subjected to a third saccharification reaction, and the resulting reaction solution is retained to obtain a third concentrate and a third filtrate. After combining the first, second, and third concentrates, decolorization and filtration were performed sequentially to obtain the crude liquid. The crude liquid is sequentially desalted, concentrated and dried to obtain a high-panose material; the panose content in the high-panose material is ≥90wt%.
2. The preparation method according to claim 1, characterized in that, The temperatures for the first, second, and third saccharification reactions are independently 50–70 °C; The holding time for the first saccharification reaction is 6-8 hours, the holding time for the second saccharification reaction is 3-4 hours, and the holding time for the third saccharification reaction is 1-5 hours.
3. The preparation method according to claim 1, characterized in that, The retention is achieved using a semi-permeable membrane; the pore size of the semi-permeable membrane is 400~500 Da.
4. The preparation method according to claim 1, characterized in that, The malt syrup contains ≤10% glucose by mass; the malt syrup has a solids content of 35-40 wt% and a pH value of 4.9-5.
5.
5. The preparation method according to claim 1, characterized in that, The mass ratio of the first filtrate to malt syrup is 1:1 to 1:3; the mass ratio of the second filtrate to malt syrup is 1:3 to 1:
6.
6. The preparation method according to claim 1 or 2, characterized in that, The amount of glucosidase added is 400~800mL / T.DS; the decolorization temperature is 75~85℃, and the holding time is 20~40min.
7. The preparation method according to claim 1, characterized in that, During the desalination process, the feed temperature of the crude liquid is 35~40℃, the feed rate is 1~3 BV / h, and the pH value of the output is 5.0~6.
0.
8. The high-panol material prepared by the preparation method according to any one of claims 1 to 7, characterized in that, The high-panose material has a panose content of ≥90wt%.
9. The use of the high-panol material prepared by the preparation method according to any one of claims 1 to 7 or the high-panol material according to claim 8 in toothpaste.
10. The application as described in claim 9, characterized in that, The amount of high-panose material added to the toothpaste is 1-8 wt%.