CN110790800A - Method for reducing impurities in crystallized maltose - Google Patents
Method for reducing impurities in crystallized maltose Download PDFInfo
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- CN110790800A CN110790800A CN201911102813.0A CN201911102813A CN110790800A CN 110790800 A CN110790800 A CN 110790800A CN 201911102813 A CN201911102813 A CN 201911102813A CN 110790800 A CN110790800 A CN 110790800A
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Abstract
The invention discloses a method for reducing impurities in crystallized maltose, and belongs to the technical field of food. The invention has simple process, does not need to invest large-scale equipment, does not have the potential safety hazard similar to alcohol, has lower material cost, greatly reduces the impurity content in the purified crystallized maltose, and shows by HPLC analysis that the impurity content before and after the main peak is lower than 0.5 percent, and the finished product after crystallization accords with the indexes of related substances of the medicinal crystallized maltose, thereby being a purification technology capable of industrial production.
Description
Technical Field
The invention relates to a method for reducing impurities in crystallized maltose, and belongs to the technical field of food.
Background
The crystalline maltose is high-purity disaccharide produced by starch or maltodextrin through the processes of liquefaction, saccharification, decoloration, ion exchange and crystallization. The maltose of the traditional production is mostly maltose syrup of 40%, 50% and 70% and crystalline maltose with the content of more than 90%, while the production difficulty of the medicinal crystalline maltose is much greater, mainly the maltose content of the massecuite before crystallization needs to be more than 92%, the viscosity of the centrifugal material is high, the difficulty of crystallization separation is high, and the impurity sugar after crystallization is too much, so the related substance index is unqualified. The related substance index of the medicinal crystalline maltose is mainly to remove the heterosugar except the maltose, and the front of the main peak is less than or equal to 1.5 percent, and the back of the main peak is less than or equal to 0.5 percent. At present, an ethanol crystallization method, a direct crystallization method, an ion exchange method, an activated carbon adsorption method and the like are used, but the problems of low safety coefficient, high operation cost, low yield, large equipment investment and the like exist.
Disclosure of Invention
The invention provides a method for reducing impurities in crystallized maltose, which is characterized in that syrup is decolorized by modified activated carbon and then subjected to ion exchange to obtain the maltose syrup with the content of 88-95%.
In one embodiment of the invention, the modified activated carbon is prepared by treating activated carbon in 5-10% ammonia water according to a mass ratio of 1: 8-10 at 50-60 ℃ for 2-3 h, washing until the pH value is 6.5-7.5, and drying at 80-100 ℃.
In one embodiment of the present invention, the modified activated carbon is added in an amount of 0.5 to 1% by mass (in terms of solid content).
In one embodiment of the invention, the ion exchange is to adopt anion and cation exchange resin, and the sugar solution is processed to the conductivity of less than or equal to 40% mu s/ms and the light transmittance of more than or equal to 99%.
It is a second object of the present invention to provide a method for industrially preparing crystalline maltose having low impurities, which comprises the steps of:
(1) decoloring the syrup by using modified activated carbon, and then performing ion exchange to obtain 88-95% maltose syrup;
(2) preparing crystalline maltose by adopting a twice crystallization method; the double crystallization method is to perform double crystallization at different temperatures.
In one embodiment, the two crystallizations are in particular: (1) the sugar feeding temperature is 50-60 ℃, the pH is 4.0-5.0, the seed amount of 0.1-3% crystal is controlled, the dry matter concentration is 70-75%, and after crystal growth is carried out for 50-72 h, centrifugal washing is carried out to obtain 95-98% crystallized maltose; (2) adding water to dissolve 97-98% of the crystals obtained in the step (1), and adding 2-3% of the crystals obtained in the step (1) as seed crystals to perform secondary crystallization, wherein the specific conditions are as follows: the sugar feeding temperature is 50-70 ℃, the pH value is 4.0-6.0, and the water washing is carried out after the crystal growth is carried out for 60-96 h.
In one embodiment of the invention, the modified activated carbon in the step (1) is prepared by treating activated carbon in 5-10% ammonia water according to a mass ratio of 1: 8-10 at 50-60 ℃ for 2-3 h, washing until the pH value is 6.5-7.5, and drying at 80-100 ℃.
In one embodiment of the invention, the ion exchange is to adopt anion and cation exchange resin, and the sugar solution is processed to the conductivity of less than or equal to 40% mu s/ms and the light transmittance of more than or equal to 99%.
In one embodiment of the invention, the method further comprises centrifuging and washing the crystals.
In one embodiment of the invention, the method also dries the washed crystal in an environment with the temperature of 100-110 ℃ and the humidity of less than or equal to 20%.
The invention also claims the application of the method in preparing food and pharmaceutical maltose.
Has the advantages that: the invention has simple process, does not need to invest large-scale equipment, does not have the potential safety hazard similar to alcohol, has lower material cost, greatly reduces the impurity content in the purified crystallized maltose, and shows by HPLC analysis that the impurity content before and after the main peak is lower than 0.5 percent, and the finished product after crystallization accords with the indexes of related substances of the medicinal crystallized maltose, thereby being a purification technology capable of industrial production.
Drawings
FIG. 1 is a chromatogram of a control sample of crystallized maltose.
FIG. 2 is a chromatogram of a crystalline maltose end product prepared herein.
Detailed Description
Example 1 preparation of modified activated carbon
Respectively placing the activated carbon in 5% ammonia water, 0.2M HCl and 0.2M H according to the mass ratio of 1:102SO4Treating at 55 deg.C for 3 hr, washing to pH 7.0, and oven drying at 90 deg.C.
The prepared activated carbon was used to treat a maltose syrup containing about 90% of the hydrolyzed maltose by using the maltogenic amylase, the activated carbon was added to the maltose syrup in an amount of 0.5% (m/m, based on the mass of the solid matter), the mixture was stirred at a low speed of 55 ℃ for 20min, and the decolorization ratio was calculated according to the following formula, and the results are shown in table 1.
Decolorization ratio (color value before decolorization-color value after decolorization)/color value before decolorization × 100%.
TABLE 1 decolorization ratio of different activated carbons
| 5% ammonia water treatment | 0.2M HCl treatment | 0.2M H2SO4Treatment of | |
| Decolorization ratio | 92.31％ | 86.87％ | 87.62％ |
Example 2 decolorization of modified activated carbon
The decolorizing performance of the modified activated carbon is optimized according to the following method:
(1) putting the activated carbon into 5% ammonia water according to the mass ratio of 1:10, treating for 3h at 55 ℃, washing until the pH value is 7.0, and drying at 90 ℃ to obtain the modified activated carbon 1.
(2) Putting the activated carbon into 10% ammonia water according to the mass ratio of 1:10, treating at 55 ℃ for 3h, washing until the pH value is 7.0, and drying at 90 ℃ to obtain modified activated carbon 2.
(3) Putting the activated carbon into 5% ammonia water according to the mass ratio of 1:5, treating for 2h at 50 ℃, washing until the pH value is 7.0, and drying at 90 ℃ to obtain modified activated carbon 3.
(4) Treating the mixture in 5% ammonia water according to the mass ratio of 1:10 at 50 ℃ for 2h, washing the mixture until the pH value is 7.0, and drying the mixture at 90 ℃ to obtain modified activated carbon 4.
The modified activated carbons 1 to 4 prepared according to the method of example 1 were added to malt syrup having about 90% content after hydrolysis with maltogenic amylase, respectively, and the results are shown in Table 2.
TABLE 2 decolorization ratio of different activated carbons
| Modified activated carbon 1 | Modified activated carbon 2 | Modified activated carbon 3 | Modified activated carbon 4 | |
| Decolorization ratio | 92.31％ | 93.15％ | 89.11％ | 95.42％ |
The inventors have also made various attempts at the temperature of the activated carbon treatment, and as a result, it was revealed that the activated carbon obtained by the treatment was not good in adsorption effect after the temperature exceeded 60 ℃.
Example 3
(1) Inactivating enzyme of the maltose syrup after enzymolysis treatment, decolorizing, adding 0.5% modified activated carbon (prepared by treating modified activated carbon in 5% ammonia water at 50 deg.C for 2 hr, washing to pH 7.0, and oven drying at 90 deg.C) at 50 deg.C for 20 min;
(2) passing the sugar solution decolorized in the step (1) through a cation exchange column and an anion exchange column in sequence to ensure that the conductivity is less than or equal to 40% mu s/ms, and entering a concentrator to concentrate until the concentration of dry matters is 75%;
(3) pumping the 92% maltose syrup obtained in the step (2) into a crystallization kettle by using a screw pump, wherein the pH of the fed material is 4.2, the initial temperature is 50 ℃, the dry matter concentration is 72%, the crystal seed amount is 0.5%, and after gradient cooling is carried out for 45 hours, pumping the maltose syrup into a centrifuge with separation factors 1008 by using the screw pump for centrifugation, wherein the specific centrifugation mode is as follows:
feeding at a rotating speed of 600r/min, uniformly distributing a certain amount of materials on a rotary drum of a centrifuge, increasing the rotating speed to 1000r/min, after 10min, reducing the rotating speed to 600r/min, starting to operate a first-step water washing program, after the water washing is finished, increasing the rotating speed to 1000r/min, starting to operate a second-step water washing program, after the water washing is finished, increasing the rotating speed to 1200r/min, discharging after 10min, and taking the centrifugal time with the water content below 10% as a standard;
(4) secondary crystallization: adding water to 97% by mass of the material crystallized in the step (3) for dissolving, wherein the pH of the fed material is 4.2, the initial temperature is 60 ℃, the dry matter concentration is 73%, adding the rest 3% of crystals in the step (3) as seed crystals, performing gradient cooling for 60 hours, and driving the seed crystals into a centrifuge with separation factors 1008 by using a screw pump for centrifugation, wherein the specific centrifugation mode is as follows:
feeding at a rotating speed of 600r/min, uniformly distributing a certain amount of materials on a rotary drum of a centrifuge, increasing the rotating speed to 1000r/min, after 10min, reducing the rotating speed to 600r/min, starting to operate a first-step water washing program, after the water washing is finished, increasing the rotating speed to 1000r/min, starting to operate a second-step water washing program, after the water washing is finished, increasing the rotating speed to 1200r/min, discharging after 10min, and centrifuging until the water content is reduced to below 10%.
The obtained product is subjected to chromatographic detection, and the result shows that the indexes of related substances of the finished product are 0.3 percent before the main peak and 0.45 percent after the main peak.
Example 4
(1) Inactivating enzyme of the maltose syrup after enzymolysis treatment, decolorizing, adding 0.5% modified activated carbon (prepared by treating modified activated carbon in 5% ammonia water at 50 deg.C for 2 hr, washing to pH 7.0, and oven drying at 90 deg.C) at 50 deg.C for 20 min;
(2) sequentially passing the sugar solution decolorized in the step (1) through a cation exchange column and an anion exchange column to ensure that the conductivity is less than or equal to 40% mu s/ms, and concentrating the sugar solution in a concentrator until the concentration of dry matters is 73%;
(3) pumping the maltose massecuite obtained in the step (2) into a crystallization kettle by using a screw pump, wherein the pH of the fed material is 5.0, the seed crystal amount is 0.8%, the initial temperature is 50 ℃, after gradient cooling is carried out for 60 hours, pumping the maltose massecuite into a centrifuge with separation factors 1008 by using the screw pump for centrifugation, and the specific centrifugation mode is as follows:
feeding at a rotating speed of 600r/min, uniformly distributing a certain amount of materials on a rotary drum of a centrifuge, increasing the rotating speed to 1000r/min, starting to operate a first-step water washing program after 10min, increasing the rotating speed to 1200r/min after the water washing is finished, starting to operate a second-step water washing program, discharging after 10min, and centrifuging for a time until the water content is reduced to below 10%.
(4) Secondary crystallization: adding 97.5% by mass of the material crystallized in the step (3) into water for dissolving, wherein the pH of the fed material is 5.0, the initial temperature is 55 ℃, the dry matter concentration is 72%, adding the rest 2.5% of crystals in the step (3) as seed crystals, performing gradient cooling for 60 hours, driving the seed crystals into a centrifuge with separation factors 1008 by using a screw pump, and centrifuging, wherein the specific centrifugation mode is as follows:
feeding at a rotating speed of 600r/min, uniformly distributing a certain amount of materials on a rotary drum of a centrifuge, increasing the rotating speed to 1000r/min, starting to operate a first-step water washing program after 10min, increasing the rotating speed to 1200r/min after the water washing is finished, starting to operate a second-step water washing program, and discharging after 10min, wherein the centrifugation time is based on the water content of less than 10%.
The obtained product is subjected to chromatographic detection, and the result shows that (shown in figure 1-2), the indexes of related substances of the finished product are 0.25% before the main peak and 0.4% after the main peak.
Example 5
(1) Inactivating enzyme of the maltose syrup after enzymolysis treatment, decolorizing, adding 0.5% modified activated carbon (prepared by treating modified activated carbon in 5% ammonia water at 50 deg.C for 2 hr, washing to pH 7.0, and oven drying at 90 deg.C) at 50 deg.C for 20 min;
(2) passing the sugar solution decolorized in the step (1) through a cation exchange column and an anion exchange column in sequence to ensure that the conductivity is less than or equal to 40% mu s/ms, and entering a concentrator to concentrate until the concentration of dry matters is 75%;
(3) pumping the maltose massecuite concentrated in the step (2) into a crystallization kettle by using a screw pump, wherein the pH of the fed material is 4.5, the initial temperature is 50 ℃, the concentration of dry matters is 75%, the seed amount is 0.3%, after gradient cooling is carried out for 72h, pumping the maltose massecuite into a centrifuge with separation factors 1008 by using the screw pump, and centrifuging, wherein the specific centrifugation mode is as follows:
feeding at a rotating speed of 600r/min, uniformly distributing a certain amount of materials on a rotary drum of a centrifuge, increasing the rotating speed to 1000r/min, after 10min, reducing the rotating speed to 600r/min, starting to operate a first-step water washing program, after the water washing is finished, increasing the rotating speed to 1000r/min, starting to operate a second-step water washing program, after the water washing is finished, increasing the rotating speed to 1200r/min, discharging after 10min, and taking the centrifugation time with the water content below 10% as a standard.
(4) Secondary crystallization: adding water to 97.5% by mass of the primary crystallized material prepared in the step (3) for dissolving, wherein the pH of the fed material is 4.5, the initial temperature is 50 ℃, the dry matter concentration is 75%, adding the rest 2.5% of crystals in the step (3) as seed crystals, performing gradient cooling for 72h, driving the seed crystals into a centrifuge with a separation factor 1008 by using a screw pump, and centrifuging, wherein the specific centrifugation mode is as follows:
feeding at a rotating speed of 600r/min, uniformly distributing a certain amount of materials on a rotary drum of a centrifuge, increasing the rotating speed to 1000r/min, after 10min, reducing the rotating speed to 600r/min, starting to operate a first-step water washing program, after the water washing is finished, increasing the rotating speed to 1000r/min, starting to operate a second-step water washing program, after the water washing is finished, increasing the rotating speed to 1200r/min, discharging after 10min, and taking the centrifugation time with the water content below 10% as a standard.
The obtained product is subjected to chromatographic detection, and the result shows that the indexes of related substances of the finished product are 0.3 percent before the main peak and 0.5 percent after the main peak.
EXAMPLE 6 extension of crystallization Cooling time
The same treatment conditions as in example 3 were adopted, except that the temperature reduction time in step (4) was increased from 60h to 72h, and compared with example 3, the crystal particles were coarser, the viscosity was reduced, and the centrifugation difficulty was reduced. The results of the final product in example 3 on the indexes of the substances are 0.30% before the main peak and 0.45% after the main peak, while the measurement results of this example are 0.10% before the main peak and 0.30% after the main peak, which effectively reduces the content of the heterosugar in the final product.
Example 5 increasing Water washing procedure
The same treatment conditions as in example 4 were adopted, except that the washing procedure was different, and a one-step washing procedure was added, and washing was carried out at 600r/min, 1000r/min, and 1200r/min, respectively, under the same washing amount. The results of the final product in example 4 on the substance indexes are 0.25% before the main peak and 0.4% after the main peak, while the results in this example are 0.05% before the main peak and 0.20% after the main peak, effectively reducing the content of the heterosugar in the final product.
Example 6 reduction of the Dry matter concentration of the feed
The same processing conditions as in example 5 were used except that the concentration of the dry matter of the feed material for crystallization was 70%, the results of the indexes of the relevant substances of the final product in example 5 were 0.3% before the main peak and 0.5% after the main peak, whereas the results in this example were 0.05% before the main peak and 0.26% after the main peak, the viscosity of the material in comparative example 3 was significantly reduced, the difficulty of centrifugation was greatly reduced, and the yield of the finished product was ensured.
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 method for reducing impurities in crystallized maltose is characterized in that the method comprises the steps of decoloring syrup by using modified activated carbon, and then performing ion exchange to obtain maltose syrup with the content of 88-95%; the modified activated carbon is prepared by treating activated carbon in 5-10% ammonia water according to the mass ratio of 1: 8-10 at 50-60 ℃ for 2-3 h, washing until the pH value is 6.5-7.5, and drying at 80-100 ℃.
2. The method according to claim 1, wherein the modified activated carbon is added in an amount of 0.5 to 1%.
3. The method as claimed in claim 1, wherein the ion exchange is carried out by treating the sugar solution with anion and cation exchange resins to obtain a solution with a conductivity of 40% μ s/ms or less and a light transmittance of 99% or more.
4. A method for industrially producing crystalline maltose having low impurities, characterized in that the method comprises the steps of:
(1) decoloring the syrup by using modified activated carbon, and then performing ion exchange to obtain 88-95% maltose syrup;
(2) preparing crystalline maltose by adopting a twice crystallization method; the twice crystallization method is to carry out twice crystallization at different temperatures; the modified activated carbon is prepared by treating activated carbon in 5-10% ammonia water according to the mass ratio of 1: 8-10 at 50-60 ℃ for 2-3 h, washing until the pH value is 6.5-7.5, and drying at 80-100 ℃.
5. The method according to claim 4, characterized in that said two crystallizations are in particular: (1) the sugar feeding temperature is 50-60 ℃, the pH is 4.0-5.0, the seed amount of 0.1-3% crystal is controlled, the dry matter concentration is 70-75%, and after crystal growth is carried out for 45-72 h, centrifugal washing is carried out to obtain the crystalline maltose with the purity of 95-98%; (2) according to the mass percent, 97-98% of the crystals obtained in the step (1) are dissolved in water, and 2-3% of the crystals obtained in the step (1) are added as seed crystals to carry out secondary crystallization, wherein the specific conditions are as follows: the sugar feeding temperature is 50-60 ℃, the pH value is 4.0-5.0, and the water washing is carried out after the crystal growth is carried out for 60-72 h.
6. The method as claimed in claim 5, wherein the modified activated carbon in the step (1) is prepared by treating activated carbon in 5-10% ammonia water according to a mass ratio of 1: 8-10 at 50-60 ℃ for 2-3 h, washing until the pH is 6.5-7.5, and drying at 80-100 ℃.
7. The method as claimed in claim 5, wherein the ion exchange is carried out by treating the sugar solution with anion and cation exchange resins to obtain a solution with a conductivity of 40% μ s/ms or less and a light transmittance of 99% or more.
8. A process according to any one of claims 5 to 7, wherein the process further comprises centrifuging and washing the crystals.
9. The method according to any one of claims 5 to 8, wherein the washed crystals are dried at 100 to 110 ℃ and a humidity of 20% or less.
10. Use of the method according to any one of claims 5 to 9 for the preparation of crystalline maltose or a product derived therefrom in the fields of food and medicine.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060084150A1 (en) * | 2004-09-29 | 2006-04-20 | Qunyu Gao | Method for manufacturing maltose-rich products |
| CN102676616A (en) * | 2012-05-16 | 2012-09-19 | 成都连接流体分离科技有限公司 | Efficient and environment-friendly malt syrup producing process |
| CN109234339A (en) * | 2018-11-22 | 2019-01-18 | 湖南汇升生物科技有限公司 | A kind of production method of high-purity crystallized maltose |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060084150A1 (en) * | 2004-09-29 | 2006-04-20 | Qunyu Gao | Method for manufacturing maltose-rich products |
| CN102676616A (en) * | 2012-05-16 | 2012-09-19 | 成都连接流体分离科技有限公司 | Efficient and environment-friendly malt syrup producing process |
| CN109234339A (en) * | 2018-11-22 | 2019-01-18 | 湖南汇升生物科技有限公司 | A kind of production method of high-purity crystallized maltose |
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| 周建斌等: ""改性活性炭对木糖液脱色性能的研究"", 《福建林学院学报》 * |
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