Patent Application
20250059225
The present application claims the priority right of the Chinese patent application No. 202111633962.7 filed on Dec. 29, 2021, which is incorporated into the text with reference in its entirety.
The disclosure belongs to the technical field of the production of saccharides, and especially, it relates to a method for preparing Stachyose.
Stachyose is a tetra-saccharide that is a white powder and slightly sweet in taste. It has a molecular formula C24H42O21, and a molecular structure of “galactose-galactose-glucose-fructose”.
Stachys affinis is a plant in Stachys Genus, Labiatae Family. The tubers of the Stachys affinis is rich in Stachyose.
The inventors find that in traditional production and preparation technologies of Stachyose, the following problems are involved:
In view of this, it is the object of the present disclosure to provide a method for preparing Stachyose, and with the method provided by the present disclosure, the Stachyose product has a high purity, a low salt content and a low electrical conductivity.
In order to achieve the above object, the present disclosure provides the following technical solution:
The disclosure provides a method for preparing Stachyose, comprising the following steps:
In some embodiments, the method for preparing Stachyose can effectively reduce electrically conductive ash content of the Stachyose, and the method for preparing Stachyose is a preparation method of effectively reducing the electrically conductive ash content in the Stachyose.
In some embodiments, a particle size of the wall-broken material in the step 1) is 3 mm to 5 mm.
In some embodiments, conditions of the filter pressuring in the step 2) include: conducting the filter pressing by using a belt pressure filter, with a pedrail mesh number of 60 meshes-80 meshes, a pressure of 0.2 Mpa-0.5 Mpa, and a temperature of not more than 30° C.
In some embodiments, conditions of the decoloring treatment in the step 3) include: conducting the decoloring treatment by using an immobilized carbon column, with a temperature of 50° C.-60° C., and a flow rate per hour of the filtrate of 0.7 times-1 time of the column volume.
In some embodiments, the nanofiltration membrane in the step 4) has a molecular weight cut-off of 300 Da.
In some embodiments, the conditions of the mixed bed ion exchange treatment in the step 5) include: a temperature of 5° C. and a flow rate per hour of the nanofiltration liquid of 2 times of a column volume.
In some embodiments, the treatment capacity of the step 6) is 0.04 kg dry basis/L resin/h.
In some embodiments, conditions of the vacuum drying in the step 7) include: a pressure of −0.09 Mpa to −0.1 Mpa, and a temperature of 65° C.-85° C.
In some embodiments, the filter residues in the step 2) are vacuum dried to obtain a byproduct vegetable protein.
In some embodiments, the conditions of the vacuum drying include: a pressure of −0.09 Mpa to −0.1 Mpa, and a temperature of 60° C.-80° C.
The present disclosure provides a method for preparing Stachyose. The present disclosure uses a nanofiltration membrane to remove salts and a part of monosaccharides in the decolorized liquid, with a desalination rate reaching more than 99.0%. The desalinated material is further treated by the means of mixed bed ion exchange, to further reduce the electric conductivity of the product, with an electric conductivity of the finished product of ≤50%, and an electrically conductive ash content of ≤0.01%, and also, the use of the mixed bed ion exchange treatment can reduce greatly the degradation of Stachyose during the ion exchange treatment and keep the purity of the Stachyose not to be reduced. The continuous simulated moving bed chromatographic separation is used to increase the purity of the product to more than 98%, reduce the contents of sucrose and other monosaccharides (glucose, fructose), and greatly improve the quality of the product, so that the product can be applied to low-sugar or low-glycemic index products. At the vacuum drying condition, the drying temperature of the material may be reduced, and the stability of Stachyose can be efficiently kept. Finally, a low-salt, low-conductivity and high-purity Stachyose is obtained.
The Stachyose prepared by using the preparation method provided by the present disclosure has an electric conductivity of 37 μs/cm-41 μs/cm, an electrically conductive ash content of 0.0091%-0.0094% and a purity of 98.92%-99.0%.
In the present application, the Stachys affinis for extracting Stachyose refers to tubers of the Stachys affinis.
In the present application, the mixed bed ion exchange treatment refers to a treatment using a mixed bed ion exchange resin. The mixed bed ion exchange resin refers to a resin containing both an anion exchange resin and a cation exchange resin. The use of the mixed bed ion exchange treatment can remove cation and anion ions in a solution simultaneously.
In the present application, the continuous simulated moving bed chromatographic purification refers to a treatment using simulated moving bed chromatography. In the simulated moving bed technology, a feeding inlet, a solvent or eluent inlet, and locations of exports for desired and undesired products, rather than a bed, are continuously moved, giving the impression that the bed is moved, solid particles continuously flow, and a liquid continuously flows in a direction opposite to that of the solid particles. The continuous simulated moving bed chromatography used in the present application is, for example, any of simulated moving bed chromatography technologies described in the following document, Lin Bingchang, Simulated Moving Bed Chromatography Technology [M], Chemical Industry Press, 2008.
In the present application, the unit “1 kg dry basis/L resin/h” means that a solution containing 1 kg dry basis is treated per liter resin per hour.
In the present application, the “electrically conductive ash content” refers to the weight percentage of substances remained after Stachyose is burnt to completely remove organic substances, relative to the sample.
In the present application, the detection standards for the purity and electrically conductive ash content of the Stachyose refer to QB/T4260-2018; the detection of the conductivity detection refers to GB/T35887-2018; the detection of the chrominance refers to the standard GB/T20881.4-2021; the detection of the light transmittance refers to GB/T20881-2017.
The drawings are illustrated here to provide further understandings to the present application and constitute a part of the present application. The schematic examples of the present disclosure and illustrations thereof are used for explaining the present disclosure, but not for limiting the present disclosure. In the following drawings:
References will now be made in detail to specific embodiments of the present disclosure. Examples of the specific embodiments are shown in the drawings. While these specific embodiments describe the present disclosure, it should be recognized that it is not intended to limit the present disclosure to these specific embodiments. In contrast, these embodiments are intended to cover alternative, modified and equivalent embodiments that are included within the inventive spirit and scope as defined by the claims. In the following descriptions, numerous specific details are elaborated to provide thorough understandings to the present disclosure. The present disclosure may be implemented without some or all of these specific details. In other instances, in order not to unnecessarily obscure the present disclosure, well known process operations are not described in detail.
The disclosure provides a method for preparing Stachyose, comprising the following steps:
The present disclosure breaks walls of Stachys affinis, to obtain a wall-broken material.
In the present disclosure, the Stachys affinis is preferably fresh Stachys affinis, which contains 75%-80% of water, 17%-20% of saccharides, 2.5%-5.5% of proteins and ≤0.3% of fat, but free of cellulose and lignin. According to the present disclosure, preferably, after the Stachys affinis is cleaned, it is subjected to a wall breaking pretreatment with a hammer-type wall breaking machine, and a screen having a pore size of 4 mm-6 mm is selected as the used wall breaking screen, to control the size of the wall-broken material to be from 3 mm to 5 mm. The size of the wall-broken material affects belt filter pressing effects. A too large size will cause the belt squeeze to have a low juice yield and a high water content in filter residues, and a too low size will result in a reduced quality of the filtrate and too much filter residues.
According to the present disclosure, the obtained wall-broken material is subjected to the filter pressing to obtain a filtrate and filter residues. In the present disclosure, the conditions of the filter pressing preferably include: conducting the filter pressing by using a belt pressure filter, with a pedrail mesh number of 60 meshes-80 meshes, a pressure of 0.2 Mpa-0.5 Mpa, and a temperature of not more than 30° C. In the present disclosure, the filter residues are preferably vacuum dried to obtain a byproduct vegetable protein, and the conditions of the vacuum drying preferably include: a pressure of −0.09 Mpa to −0.1 Mpa, and a temperature of 60° C. to 80° C.
According to the present disclosure, the obtained filtrate is decolorized to obtain decolorized liquid. In the present disclosure, the conditions of the decoloring treatment preferably include: conducting the decoloring treatment by using an immobilized carbon column, with a temperature of 50° C.-60° C., and a flow rate per hour of the filtrate of 0.7 times-1 time of the column volume.
According to the present disclosure, the obtained decolorized liquid is subjected to a nanofiltration membrane filtration, to obtain a nanofiltration liquid; the conditions of the nanofiltration membrane filtration preferably include: a molecular weight cut-off of the nanofiltration membrane of 100 Da to 500 Da, a temperature of 30° C. to 40° C., and a pressure of 0.35 Mpa to 1 Mpa. In the present disclosure, the nanofiltration membrane preferably has a molecular weight cut-off of 300 Da. In the present disclosure, the nanofiltration membrane is adopted to remove salts and a part of monosaccharides in the decolorized liquid, with a desalination rate reaching more than 99.0%.
According to the present disclosure, the obtained nanofiltration liquid is subjected to a mixed bed ion exchange treatment, to obtain an exchanged liquid; the conditions of the mixed bed ion exchange treatment include: a temperature of 20° C. to 30° C., and a flow rate per hour of the nanofiltration liquid of 1.5 times to 2.5 times of a column volume. In the present disclosure, the conditions of the mixed bed ion exchange treatment preferably include: a temperature of 25° C., and a flow rate per hour of the nanofiltration liquid of 2.0 times of a column volume. The mixed bed ion exchange treatment is used to reduce the electric conductivity of the product, with an electric conductivity of the finished product of ≤50%, and an electrically conductive ash content of ≤0.01%, and also, the use of the mixed bed ion exchange treatment can greatly reduce the degradation of Stachyose during the ion exchange treatment and keep the purity of the Stachyose not to be reduced.
According to the present disclosure, the obtained exchanged liquid is purified by means of continuous simulated moving bed chromatography, to obtain a purified liquid; the conditions of the continuous simulated moving bed chromatography include a feeding concentration of 50% to 55%, a temperature of 45° C. to 50° C., a water to material ratio of 1.5:1 to 2:1, and a treatment capacity of 0.035 kg dry basis/L resin/h to 0.045 kg dry basis/L resin/h. In the present disclosure, the treatment capacity is preferably 0.04 kg dry basis/L resin/h. The continuous simulated moving bed chromatographic separation is used to increase the purity of the product to more than 98%, reduce the contents of sucrose and other monosaccharides (glucose, fructose), and greatly improve the quality of the product quality, so that the product can be applied to low-sugar or low-glycemic index products.
According to the present disclosure, the obtained purified liquid is concentrated and vacuum dried, to obtain Stachyose. In the present disclosure, the conditions of the vacuum drying include: a pressure of −0.09 Mpa to −0.1 Mpa, and a temperature of 65° C. to 85° C. According to the present disclosure, a vacuum belt dryer is preferably used to vacuum dry the product. At the vacuum conditions, the drying temperature of the material may be reduced, and the stability of the Stachyose can be efficiently kept. The present disclosure does not specially limit the conditions of the concentrating, and routine conditions may be used.
The concentrations mentioned in the present disclosure each are mass concentrations.
In order to further illustrate the present disclosure, the following examples are combined to describe the present disclosure in detail, but they should not be construed as limiting the protection scope of the disclosure.
According to the above operation steps, the results are shown below:
According to the above operation steps, the results are shown below:
Comparative Examples 1-2 differed from Example 1 in the parameter settings of the continuous simulated moving bed chromatography. The differences in the continuous simulated moving bed parameter settings between Comparative Examples 1-2 and Example 1 were shown below:
As mentioned above, after the product purified by continuous simulated moving bed chromatography in Example 1 was vacuum dried at low temperatures, a stachyose finished product was obtained, with a purity of the finished product of 98.67%, an electrically conductive ash content of 0.0091%, an electric conductivity of 37 μs/cm, a chrominance of 8.00, and a light transmittance of 99.0%.
After the product purified by continuous simulated moving bed chromatography in Comparative Example 1 was vacuum dried at low temperatures, a stachyose finished product was obtained, with a purity of the finished product of 94.37%, an electrically conductive ash content of 0.0101%, an electric conductivity of 53 μs/cm, a chrominance of 10.34, and a light transmittance of 99.0%. Comparative Example 1 was inferior to Example 1.
After the product purified by continuous simulated moving bed chromatography in Comparative Example 2 was vacuum dried at low temperatures, a stachyose finished product was obtained, with a purity of the finished product of 97.48%, an electrically conductive ash content of 0.0099%, an electric conductivity of 47 μs/cm, a chrominance of 9.62, and a light transmittance of 98.9%. Comparative example 2 was inferior to Example 1.
In Comparative Example 1, the feeding concentration, temperature and water to material ratio of the continuous simulated moving bed chromatography were lower than the ranges in the technical solution of the present disclosure (that is, the feeding concentration: 50-55%, the temperature: 45-50° C., and the water to material ratio: 1.5-2:1), and the stachyose product obtained in Comparative Example 1 was inferior to that of Example 1 in terms of the property parameters like purity, electric conductivity, etc.
In Comparative Example 2, the feeding concentration, temperature and water to material ratio of the continuous simulated moving bed chromatography were higher than the ranges in the technical solution of the present disclosure (that is, the feeding concentration: 50-55%, the temperature: 45-50° C., and the water to material ratio: 1.5-2:1), and the stachyose product obtained in Comparative Example 2 was inferior to that of Example 1 in terms of the property parameters like purity, electric conductivity, etc.
As can be seen from this, Examples 1-2 in the present disclosure use specific continuous simulated moving bed chromatographic parameters to effectively improve the quality of the stachyose product, particularly to reduce the electrically conductive ash content of the stachyose, and they achieve significant unexpected technical effects.
While the present application has been described with reference to preferred examples, without departing from the scope of the present application, various modifications may be made and equivalents may be used to replace elements therein. Especially, as long as there is no structural conflict, the respective technical features mentioned in the respective examples may be combined in any way. The present application is not be limited to the specific examples disclosed herein, but includes all technical solutions falling within the scope of the claims.
| Number | Date | Country | Kind |
|---|---|---|---|
| 202111633962.7 | Dec 2021 | CN | national |
| Filing Document | Filing Date | Country | Kind |
|---|---|---|---|
| PCT/CN2022/142234 | 12/27/2022 | WO |
