CN113583061A - Preparation method of maltooligosaccharide glucoside - Google Patents
Preparation method of maltooligosaccharide glucoside Download PDFInfo
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- CN113583061A CN113583061A CN202110940408.7A CN202110940408A CN113583061A CN 113583061 A CN113583061 A CN 113583061A CN 202110940408 A CN202110940408 A CN 202110940408A CN 113583061 A CN113583061 A CN 113583061A
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- C07H1/06—Separation; Purification
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- C07—ORGANIC CHEMISTRY
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- C07H1/00—Processes for the preparation of sugar derivatives
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- C07H1/08—Separation; Purification from natural products
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- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/02—Acyclic radicals, not substituted by cyclic structures
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Abstract
The invention discloses a preparation method of maltooligosaccharide glucoside. In the invention, 300-400 parts of barley is weighed, 150-200 parts of phosphate buffer solution is added, and then the mixture is added into a stirring reaction kettle and mechanically stirred for 15 hours; centrifuging the prepared glucoside D mixed solution added with the catalyst, dissolving the precipitate in distilled water, taking glucoside E mixed solution, taking out maltooligosaccharide glucoside when the volume of the glucoside solution in the dialysis bag is 1/4, storing the prepared maltooligosaccharide glucoside, and finishing the whole process, wherein 2-ethylhexanol and a triacid catalyst are added when the glucoside is prepared, and the mixture is fully mixed with the mixed solution with the saturation of 80%; therefore, the reaction speed can be accelerated, the glucoside precipitation speed is increased, the subsequent production speed is increased, the labor burden is reduced for factory production, the yield is increased, and more economic benefits are brought to manufacturers.
Description
Technical Field
The invention belongs to the technical field of glucoside preparation, and particularly relates to a preparation method of maltooligosaccharide glucoside.
Background
Glucoside is a glycoside having glucose as a sugar component. Are structures having various ligands bonded to a glucose-reducing group, and such compounds are collectively called glucosides. As the ligand, there are alcohols (e.g., methyl glucoside of radish leaves); phenol (hydroquinone glucoside of leaves); isothiocyanates (e.g., potassium erucate glucosinolate from mustard seed and behenic rootstock); coumarins (e.g., isocoumarin glucoside of dichroa febrifuga); flavones (e.g., cherry flavone glycosides from cherry bark); many kinds of glucosides such as anthocyanin (e.g., anthocyanin of rose pigment) are distributed in the natural world.
However, the conventional maltooligosaccharide glucoside is produced at a slower rate, resulting in a lower yield
Disclosure of Invention
The invention aims to: in order to solve the above-mentioned problems, a method for producing maltooligosaccharide glucoside is provided.
The technical scheme adopted by the invention is as follows: a method for preparing a maltooligosaccharide glucoside, comprising the steps of:
s1, weighing 300-400 parts of barley, adding 150-200 parts of phosphate buffer solution, adding the mixture into a stirring reaction kettle, and mechanically stirring for 15 hours;
s2, after the stirring in the step S1 is finished, the centrifugal operation is started to the mixture;
s3 after S2, discarding the precipitate generated in the centrifugation process to obtain the supernatant as the crude glucoside liquid of malt, numbered glucoside A;
s4, adding 900 to 1200 parts of acetone into the glucoside A solution prepared in the step S3, shaking, standing, precipitating the mixture, and numbering the mixture as glucoside B;
s5, taking the glucoside B mixed solution from the centrifuge and keeping the temperature, adding the glucoside B mixed solution into the centrifuge, and beginning to centrifuge the glucoside B mixed solution;
s6 discarding the supernatant of the glucoside B mixed solution after the centrifugation in the step S5 and allowing the precipitate to be dissolved in distilled water, numbered glucoside C;
s7 adding glucoside C mixture solution while adding solid (NH)4)2SO4While stirring the solution, (NH) was measured4)2SO4To 30% saturation, the addition of solid (NH) is stopped4)2SO4Numbered glucoside D;
s8, centrifuging the glucoside D mixed solution prepared in the step S7;
s9 discarding the supernatant of the glucoside D mixture solution after centrifugation in step S8, and fixing the solid (NH)4)2SO4While stirring the solution, (NH) was measured4)2SO4When 80% saturation is reached, the addition of solid (NH) is stopped4)2SO4;
S10, adding 2-ethylhexanol and a three-way acid catalyst into the solution obtained in the step S9, and fully mixing the solution with a mixed solution with the saturation of 80%;
s11, centrifuging the catalyst-added glucoside D mixture solution prepared in the step S9 and dissolving the precipitate in distilled water, numbered glucoside E;
s12, taking the glucoside E mixed solution, dialyzing at 4 ℃ for 20 hours, and then performing reverse osmosis concentration;
s13, taking out the final maltooligosaccharide glucoside when the volume of glucoside liquid in the dialysis bag in the step S11 is 1/4, and storing the maltooligosaccharide glucoside; .
In a preferred embodiment, in step S1, the pH of the phosphate buffer is adjusted to 7.0, and the phosphate buffer is added and incubated at 35 ℃ for 3.5 hours.
In a preferred embodiment, in step S2, the temperature of centrifugation during centrifugation is controlled to 10 ℃, the speed of centrifugation is controlled to 1000xg, and the time of centrifugation is controlled to 35 min.
In a preferred embodiment, in step S5, the temperature of centrifugation during centrifugation is controlled to 5 ℃, the speed of centrifugation is controlled to 1000xg, and the time of centrifugation is controlled to 30 min.
In a preferred embodiment, in step S8, the temperature of centrifugation during centrifugation is controlled at 8 ℃, the speed of centrifugation is controlled at 1500xg, and the time of centrifugation is controlled at 60 min.
In a preferred embodiment, in step S11, the reverse osmosis concentration is performed by placing the dialysis bag in a plastic cup, and covering the dialysis bag with 30g of ammonium sulfate solid.
In a preferred embodiment, in the step S10, the reaction temperature after the 2-ethylhexanol and the triacid catalyst are added is controlled to 95 ℃, and the vacuum degree is controlled to 0.07 to 0.08 MPa.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
in the invention, when glucoside is prepared, 2-ethylhexanol and a three-way acid catalyst are added to be fully mixed with a mixed solution with the saturation of 80 percent; therefore, the reaction speed can be accelerated, the glucoside precipitation speed is increased, the subsequent production speed is increased, the labor burden is reduced for factory production, the yield is increased, and more economic benefits are brought to manufacturers.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a method for preparing maltooligosaccharide glucoside, which comprises the following steps:
s1, weighing 300 parts of barley, adding 150 parts of phosphate buffer solution, adding the mixture into the stirring reaction kettle, and mechanically stirring for 15 hours.
And S2, after the stirring is finished in the step S1, the centrifugal operation is started on the mixture, and in the step S2, the centrifugal temperature is controlled to be 10 ℃, the centrifugal speed is controlled to be 1000Xg, and the centrifugal time is controlled to be 35 min.
S3 after S2 is completed, the precipitate produced during centrifugation is discarded to obtain a supernatant as a malt crude glucoside solution, numbered glucoside A.
S4, adding 900-1200 parts of acetone into the glucoside A solution prepared in the step S3, shaking, standing and precipitating the mixture, wherein the number of the mixture is glucoside B.
S5, taking the glucoside B mixed solution from the centrifuge and keeping the temperature, adding the glucoside B mixed solution into the centrifuge, and beginning to centrifuge the glucoside B mixed solution; in step S5, the temperature of centrifugation is controlled at 5 deg.C, the speed of centrifugation is controlled at 1000Xg, and the time of centrifugation is controlled at 30 min.
S6-discard the supernatant of the glucoside B mixed solution after the centrifugation in the step S5 and dissolve the precipitate in distilled water, numbered glucoside C.
S7 adding glucoside C mixture solution while adding solid (NH)4)2SO4While stirring the solution, (NH) was measured4)2SO4To 30% saturation, the addition of solid (NH) is stopped4)2SO4Numbered glucoside D.
S8, the glucoside D mixture solution prepared in the step S7 is centrifuged, and in the step S8, the temperature of centrifugation is controlled at 8 ℃, the speed of centrifugation is controlled at 1500Xg, and the time of centrifugation is controlled at 60 min.
S9 discarding the supernatant of the glucoside D mixture solution after centrifugation in step S8, and fixing the solid (NH)4)2SO4While stirring the solution, (NH) was measured4)2SO4When 80% saturation is reached, the addition of solid (NH) is stopped4)2SO4。
S10, adding 2-ethylhexanol and a three-way acid catalyst to the mixture obtained in the step S9, and mixing the mixture with a mixed solution having a saturation of 80%. In the step S10, the reaction temperature is controlled to be 95 ℃ after the 2-ethyl hexanol and the tribasic acid catalyst are added, and the vacuum degree is controlled to be 0.07-0.08 MPa.
S11, the catalyst-added glucoside D mixture solution prepared in the step S9 is centrifuged, and the precipitate is dissolved in distilled water, numbered glucoside E. In step S1, the pH of the phosphate buffer was adjusted to 7.0, and the added phosphate buffer was incubated at 35 ℃ for 3.5 hours. In step S11, reverse osmosis concentration was performed by placing the dialysis bag in a plastic cup, and covering the bag with 30g of ammonium sulfate solids.
S12, the glucoside E mixed solution is dialyzed at 4 ℃ for 20 hours and then is subjected to reverse osmosis concentration.
S13, when the volume of glucoside liquid in the dialysis bag in the step S11 is 1/4, taking out the finally obtained maltooligosaccharide glucoside, and storing the obtained maltooligosaccharide glucoside so as to finish the whole process, wherein when the glucoside is prepared, 2-ethylhexanol and a three-way acid catalyst are added so as to be fully mixed with the mixed solution with the saturation of 80%; therefore, the reaction speed can be accelerated, the glucoside precipitation speed is increased, the subsequent production speed is increased, the labor burden is reduced for factory production, the yield is increased, and more economic benefits are brought to manufacturers.
Example two:
a method for preparing maltooligosaccharide glucoside, which comprises the following steps:
s1, weighing 400 parts of barley, adding 200 parts of phosphate buffer solution, adding the mixture into a stirring reaction kettle, and mechanically stirring for 15 hours.
And S2, after the stirring is finished in the step S1, the centrifugal operation is started on the mixture, and in the step S2, the centrifugal temperature is controlled to be 10 ℃, the centrifugal speed is controlled to be 1000Xg, and the centrifugal time is controlled to be 35 min.
S3 after S2 is completed, the precipitate produced during centrifugation is discarded to obtain a supernatant as a malt crude glucoside solution, numbered glucoside A.
S4, adding 900-1200 parts of acetone into the glucoside A solution prepared in the step S3, shaking, standing and precipitating the mixture, wherein the number of the mixture is glucoside B.
S5, taking the glucoside B mixed solution from the centrifuge and keeping the temperature, adding the glucoside B mixed solution into the centrifuge, and beginning to centrifuge the glucoside B mixed solution; in step S5, the temperature of centrifugation is controlled at 5 deg.C, the speed of centrifugation is controlled at 1000Xg, and the time of centrifugation is controlled at 30 min.
S6-discard the supernatant of the glucoside B mixed solution after the centrifugation in the step S5 and dissolve the precipitate in distilled water, numbered glucoside C.
S7 adding glucoside C mixture solution while adding solid (NH)4)2SO4While stirring the solution, (NH) was measured4)2SO4To 30% saturation, the addition of solid (NH) is stopped4)2SO4Numbered glucoside D.
S8, the glucoside D mixture solution prepared in the step S7 is centrifuged, and in the step S8, the temperature of centrifugation is controlled at 8 ℃, the speed of centrifugation is controlled at 1500Xg, and the time of centrifugation is controlled at 60 min.
S9 discarding the supernatant of the glucoside D mixture solution after centrifugation in step S8, and fixing the solid (NH)4)2SO4While stirring the solution, (NH) was measured4)2SO4When 80% saturation is reached, the addition of solid (NH) is stopped4)2SO4。
S10, adding 2-ethylhexanol and a three-way acid catalyst into the solution obtained in the step S9, and fully mixing the solution with a mixed solution with the saturation of 80%; in the step S10, the reaction temperature is controlled to be 95 ℃ after the 2-ethyl hexanol and the tribasic acid catalyst are added, and the vacuum degree is controlled to be 0.07-0.08 MPa.
S11, the catalyst-added glucoside D mixture solution prepared in the step S9 is centrifuged, and the precipitate is dissolved in distilled water, numbered glucoside E. In step S1, the PH of the phosphate buffer is adjusted to 7.0, and the added phosphate buffer is incubated at 35 ℃ for 3.5 hours; in step S11, reverse osmosis concentration was performed by placing the dialysis bag in a plastic cup, and covering the bag with 30g of ammonium sulfate solids.
S12, the glucoside E mixed solution is dialyzed at 4 ℃ for 20 hours and then is subjected to reverse osmosis concentration.
S13, when the volume of glucoside liquid in the dialysis bag in the step S11 is 1/4, taking out the finally obtained maltooligosaccharide glucoside, and storing the obtained maltooligosaccharide glucoside so as to finish the whole process, wherein when the glucoside is prepared, 2-ethylhexanol and a three-way acid catalyst are added so as to be fully mixed with the mixed solution with the saturation of 80%; therefore, the reaction speed can be accelerated, the glucoside precipitation speed is increased, the subsequent production speed is increased, the labor burden is reduced for factory production, the yield is increased, and more economic benefits are brought to manufacturers.
Example three:
a method for preparing maltooligosaccharide glucoside, which comprises the following steps:
s1, 350 parts of barley is weighed, 180 parts of phosphate buffer solution is added, and then the mixture is added into a stirring reaction kettle and is mechanically stirred for 15 hours.
And S2, after the stirring is finished in the step S1, the centrifugal operation is started on the mixture, and in the step S2, the centrifugal temperature is controlled to be 10 ℃, the centrifugal speed is controlled to be 1000Xg, and the centrifugal time is controlled to be 35 min.
S3 after S2 is completed, the precipitate produced during centrifugation is discarded to obtain a supernatant as a malt crude glucoside solution, numbered glucoside A.
S4, adding 900-1200 parts of acetone into the glucoside A solution prepared in the step S3, shaking, standing and precipitating the mixture, wherein the number of the mixture is glucoside B.
S5, taking the glucoside B mixed solution from the centrifuge and keeping the temperature, adding the glucoside B mixed solution into the centrifuge, and beginning to centrifuge the glucoside B mixed solution; in step S5, the temperature of centrifugation is controlled at 5 deg.C, the speed of centrifugation is controlled at 1000Xg, and the time of centrifugation is controlled at 30 min.
S6-discard the supernatant of the glucoside B mixed solution after the centrifugation in the step S5 and dissolve the precipitate in distilled water, numbered glucoside C.
S7 adding glucoside C mixture solution while adding solid (NH)4)2SO4While stirring the solution, (NH) was measured4)2SO4To 30% saturation, the addition of solid (NH) is stopped4)2SO4Numbered glucoside D.
S8, the glucoside D mixture solution prepared in the step S7 is centrifuged, and in the step S8, the temperature of centrifugation is controlled at 8 ℃, the speed of centrifugation is controlled at 1500Xg, and the time of centrifugation is controlled at 60 min.
S9 discarding the supernatant of the glucoside D mixture solution after centrifugation in step S8, and fixing the solid (NH)4)2SO4While stirring the solution, (NH) was measured4)2SO4When 80% saturation is reached, the addition of solid (NH) is stopped4)2SO4。
S10, adding 2-ethylhexanol and a three-way acid catalyst into the solution obtained in the step S9, and fully mixing the solution with a mixed solution with the saturation of 80%; in the step S10, the reaction temperature is controlled to be 95 ℃ after the 2-ethyl hexanol and the tribasic acid catalyst are added, and the vacuum degree is controlled to be 0.07-0.08 MPa.
S11, the catalyst-added glucoside D mixture solution prepared in the step S9 is centrifuged, and the precipitate is dissolved in distilled water, numbered glucoside E. In step S1, the PH of the phosphate buffer is adjusted to 7.0, and the added phosphate buffer is incubated at 35 ℃ for 3.5 hours; in step S11, reverse osmosis concentration was performed by placing the dialysis bag in a plastic cup, and covering the bag with 30g of ammonium sulfate solids.
S12, the glucoside E mixed solution is dialyzed at 4 ℃ for 20 hours and then is subjected to reverse osmosis concentration.
S13, when the volume of glucoside liquid in the dialysis bag in the step S11 is 1/4, taking out the finally obtained maltooligosaccharide glucoside, and storing the obtained maltooligosaccharide glucoside so as to finish the whole process, wherein when the glucoside is prepared, 2-ethylhexanol and a three-way acid catalyst are added so as to be fully mixed with the mixed solution with the saturation of 80%; therefore, the reaction speed can be accelerated, the glucoside precipitation speed is increased, the subsequent production speed is increased, the labor burden is reduced for factory production, the yield is increased, and more economic benefits are brought to manufacturers.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. A method for producing maltooligosaccharide glucoside, comprising: the preparation method of the maltooligosaccharide glucoside comprises the following steps:
s1, weighing 300-400 parts of barley, adding 150-200 parts of phosphate buffer solution, adding the mixture into a stirring reaction kettle, mechanically stirring for 15 hours,
s2, after the stirring is finished in the step S1, the centrifugal operation of the mixture is started,
s3 after S2, discarding the precipitate generated in the centrifugation process to obtain the supernatant as the crude glucoside liquid of malt, numbered glucoside A;
s4, adding 900 to 1200 parts of acetone into the glucoside A solution prepared in the step S3, shaking, standing, precipitating the mixture, and numbering the mixture as glucoside B;
s5, taking the glucoside B mixed solution from the centrifuge and keeping the temperature, adding the glucoside B mixed solution into the centrifuge, and beginning to centrifuge the glucoside B mixed solution;
s6 discarding the supernatant of the glucoside B mixed solution after the centrifugation in the step S5 and allowing the precipitate to be dissolved in distilled water, numbered glucoside C;
s7 adding glucoside C mixture solution while adding solid (NH)4)2SO4While stirring the solution, (NH) was measured4)2SO4To 30% saturation, the addition of solid (NH) is stopped4)2SO4Numbered glucoside D;
s8, centrifuging the glucoside D mixed solution prepared in the step S7;
s9-discarding the supernatant of the glucoside D mixture solution after the centrifugation in the step S8, stirring the solution while adding solids (NH4)2SO4, when it is determined that (NH4)2SO4To 80% saturation, the addition of solid (NH4) was stopped2SO4;
S10, adding 2-ethylhexanol and a three-way acid catalyst into the solution obtained in the step S9, and fully mixing the solution with a mixed solution with the saturation of 80%;
s11, centrifuging the catalyst-added glucoside D mixture solution prepared in the step S9 and dissolving the precipitate in distilled water, numbered glucoside E;
s12, taking the glucoside E mixed solution, dialyzing at 4 ℃ for 20 hours, and then performing reverse osmosis concentration;
s13, when the volume of the glucoside liquid in the dialysis bag in the step S11 is 1/4, the maltooligosaccharide glucoside is finally obtained and stored.
2. The method for producing maltooligosaccharide glucoside of claim 1, wherein: in step S1, the PH of the phosphate buffer was adjusted to 7.0, and the added phosphate buffer was incubated at 35 ℃ for 3.5 hours.
3. The method for producing maltooligosaccharide glucoside of claim 1, wherein: in step S2, the temperature of centrifugation is controlled to 10 ℃, the speed of centrifugation is controlled to 1000xg, and the time of centrifugation is controlled to 35 min.
4. The method for producing maltooligosaccharide glucoside of claim 1, wherein: in step S5, the temperature of centrifugation is controlled at 5 ℃, the speed of centrifugation is controlled at 1000xg, and the time of centrifugation is controlled at 30 min.
5. The method for producing maltooligosaccharide glucoside of claim 1, wherein: in step S8, the temperature of centrifugation is controlled at 8 ℃, the speed of centrifugation is controlled at 1500xg, and the time of centrifugation is controlled at 60 min.
6. The method for producing maltooligosaccharide glucoside of claim 1, wherein: in step S11, the reverse osmosis concentration operation is performed by placing the dialysis bag in a plastic cup, and covering the dialysis bag with 30g of ammonium sulfate solid.
7. The method for producing maltooligosaccharide glucoside of claim 1, wherein: in the step S10, the reaction temperature is controlled to be 95 ℃ after the 2-ethyl hexanol and the tribasic acid catalyst are added, and the vacuum degree is controlled to be 0.07-0.08 MPa.
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