CN112759666B - Preparation method of semen cassiae-derived galactomannan - Google Patents
Preparation method of semen cassiae-derived galactomannan Download PDFInfo
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- CN112759666B CN112759666B CN202011555774.2A CN202011555774A CN112759666B CN 112759666 B CN112759666 B CN 112759666B CN 202011555774 A CN202011555774 A CN 202011555774A CN 112759666 B CN112759666 B CN 112759666B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/87—Re-use of by-products of food processing for fodder production
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Abstract
The invention provides a preparation method of galactomannan from cassia seed, which comprises the following steps of drying and crushing a cassia seed raw material to obtain raw material coarse powder; dispersing the raw material coarse powder in water to obtain raw material coarse liquid; centrifuging the raw material crude liquid, and dispersing the supernatant obtained by centrifuging into an alcohol extract to obtain an alcohol extract mixed solution; and centrifuging the alcohol mixed solution to obtain a precipitate, namely the galactomannan. The preparation method of the cassia seed source galactomannan takes the crushed raw material coarse powder of the cassia seed as the raw material, can simplify the step of extracting the galactomannan, has higher yield of the galactomannan, and reduces the waste of the galactomannan.
Description
Technical Field
The invention belongs to the technical field of polysaccharide preparation, and particularly relates to a preparation method of semen cassiae-derived galactomannan.
Background
The cassia seeds are seeds of cassia seeds, are rich in polysaccharide, are mainly galactomannan, and can be used as a good food additive for thickening and emulsifying. In the prior art, the method for preparing galactomannan by using cassia seeds as raw materials mainly adopts an alcohol precipitation method. However, because the galactomannans with different molecular weights have different polarities, the conventional alcohol precipitation method is difficult to extract and purify the galactomannans with different molecular weights together, thereby causing the yield of the galactomannans to be low. And the mode of extracting galactomannan by carrying out alcohol precipitation by stages by adopting reagents with different concentrations and different polarities not only has complex operation steps, but also is easy to cause reagent waste.
In view of this, a method for preparing galactomannan from cassia seeds is urgently needed to be provided at present, so that the extraction steps of galactomannan are simplified, the yield of galactomannan is higher, and the waste of galactomannan is reduced.
Disclosure of Invention
The invention aims to provide a preparation method of semen cassiae-derived galactomannan, which at least solves the technical problems of low yield of galactomannan, complex extraction operation steps and serious reagent waste in the prior art.
In order to solve the above problems, the present invention provides a method for preparing a cassia seed-derived galactomannan, comprising the steps of:
(1) drying semen Cassiae, and pulverizing to obtain coarse powder;
(2) dispersing the raw material coarse powder in the step (1) in water to obtain raw material coarse liquid;
(3) centrifuging the raw material crude liquid in the step (2), and dispersing the supernatant obtained by centrifugation into an alcohol extract to obtain an alcohol extract mixture;
(4) and (4) centrifuging the alcohol extraction mixed solution in the step (3) to obtain a precipitate, namely the galactomannan.
Preferably, the cassia seeds are crushed into particles with the particle size of less than or equal to 0.12mm in the step (1).
Preferably, the cassia seed is dried in the step (1) to be one of vacuum freeze drying, microwave drying and drying.
Preferably, in the step (2), every 1kg of raw meal is dispersed in 2-3L of water.
Preferably, in the step (3), per 100ml of the alcohol extract, the following components are included:
40ml of ethanol with the volume percentage of 35 percent to 40 percent;
40ml of isopropanol with the volume percentage of 20-25 percent;
n-amyl alcohol 10ml with volume percentage of 5% -10%;
8-12g of settling agent;
the balance being water.
Preferably, the amount of the precipitation aid is 10g per 100ml of the alcohol extract.
Preferably, the precipitation aid is poloxamer and polyacrylamide according to the weight ratio of 1: (2-10) by weight ratio.
Preferably, the settling agent is poloxamer and polyacrylamide according to the weight ratio of 1: 6 by weight ratio.
Preferably, step (3) is specifically as follows: and (3) centrifuging the raw material crude liquid in the step (2), dispersing the supernatant obtained by centrifugation into the alcohol extract, uniformly stirring, and standing for 1-3h to obtain the alcohol extract.
Preferably, in the step (3), the volume ratio of the raw material crude liquid to the alcohol extract is 1: 1.
Preferably, the step (4) further comprises a step of drying the obtained precipitate.
Compared with the prior art, the invention has the advantages and beneficial effects that:
(1) the preparation method of the cassia seed-derived galactomannan takes crushed raw material coarse powder of cassia seed as a raw material, the raw material coarse powder is dispersed in water to obtain raw material coarse liquid, and supernatant obtained by centrifugation is dispersed in alcohol extract to obtain alcohol extract mixed liquid; and finally, centrifuging the alcohol extract to obtain a precipitate, namely the galactomannan. Therefore, the extraction of the galactomannan is realized, the extraction step is simple, the yield of the galactomannan is high, and the waste of the galactomannan is reduced.
(2) The preparation method of the semen cassiae source galactomannan of the invention comprises 40ml of ethanol with 35-40% of volume percentage, 40ml of isopropanol with 20-25% of volume percentage, 10ml of n-amyl alcohol with 5-10% of volume percentage and 8-12g of precipitation aid. Isopropanol is less polar than ethanol and allows more galactomannan to settle more quickly, especially galactomannan with high molecular weight but too high a concentration of isopropanol can result in poor homogeneity of the alcoholic extract and thus reduced yield of galactomannan. The n-amyl alcohol is a medium polar solvent, and can promote the sedimentation of the galactomannan by matching with the isopropanol and the ethanol, and a good sedimentation effect can be achieved without overhigh concentration of the isopropanol. In addition, the galactomannan has large and small molecular weight, the galactomannan with large molecular weight has low polarity and poor water solubility, the galactomannan with small molecular weight has large polarity and good water solubility, the single alcohol solvent can not achieve the effect of completely settling the galactomannan with different molecular weight, and the combination of the isopropanol, the ethanol and the n-amyl alcohol can obviously improve the yield of the galactomannan.
(3) The preparation method of the semen cassiae source galactomannan provided by the invention is characterized in that the precipitation aid in the alcohol extract is poloxamer and polyacrylamide according to the weight ratio of 1: (2-10) by weight ratio. The polyacrylamide is a linear organic high molecular polymer, and can play a role in bridging among galactomannan particles in the alcohol extract, so that fine particles form larger floccules, the precipitation speed is accelerated, the galactomannan is more thoroughly precipitated, and the raw material loss is reduced. However, the endosperm of the raw material semen cassiae contains not only galactomannan but also endogenous enzymes, most of the enzymes are proteins, the proteins are macromolecules, and the macromolecules are dissolved in water to form a macromolecular solution, so that the viscosity of the alcohol extract is increased, and the alcohol extract is easy to settle under the action of polyacrylamide. The poloxamer is polyoxyethylene polyoxypropylene ether block copolymer, is a high-molecular nonionic surfactant, can dissolve impurities such as endogenous enzyme and the like in water, and can be left in a supernatant after an alcohol precipitation process, so that the purity of the galactomannan is improved.
Detailed Description
Those not indicated in the examples of the present invention were carried out under the conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by manufacturers, but are conventional products which can be obtained commercially, and the implementation of the technical scheme and the realization of the technical effect are not influenced by the raw materials of different manufacturers and models.
Example 1
The preparation method of the cassia seed-derived galactomannan of the embodiment comprises the following steps:
(1) drying semen Cassiae, and pulverizing into particles with particle diameter of 0.12mm or less to obtain coarse powder; the drying of semen Cassiae may be one of vacuum freeze drying, microwave drying, and oven drying.
(2) Dispersing the raw material coarse powder in the step (1) in 3L of water according to the proportion of 1kg of raw material coarse powder to obtain raw material coarse liquid;
(3) and (3) centrifuging the raw material crude liquid in the step (2), dispersing the supernatant obtained by centrifugation into the alcohol extract, uniformly stirring, and standing for 1h to obtain the alcohol extract. The volume ratio of the raw material crude liquid to the alcohol extract is 1: 1.
Wherein, every 100ml of the alcohol extract comprises the following components: 40ml of 35 percent ethanol by volume; 40ml of isopropanol with the volume percentage of 25 percent; 10% by volume of n-pentanol (10 ml); 8g of settling agent; the balance being water. The settling agent is poloxamer and polyacrylamide according to the weight ratio of 1: 8 by weight ratio.
(4) And (4) centrifuging the alcohol extraction mixed solution in the step (3), and drying the obtained precipitate to obtain the galactomannan.
Example 2
The preparation method of the cassia seed-derived galactomannan of the embodiment comprises the following steps:
(1) drying semen Cassiae, and pulverizing into particles with particle diameter of 0.12mm or less to obtain coarse powder; the drying of semen Cassiae may be one of vacuum freeze drying, microwave drying, and oven drying.
(2) Dispersing the raw material coarse powder in the step (1) in 2L of water according to the proportion of 1kg of raw material coarse powder to obtain raw material coarse liquid;
(3) and (3) centrifuging the raw material crude liquid in the step (2), dispersing the supernatant obtained by centrifugation into the alcohol extract, uniformly stirring, and standing for 2 hours to obtain the alcohol extract. The volume ratio of the raw material crude liquid to the alcohol extract is 1: 1.
Wherein, every 100ml of the alcohol extract comprises the following components: 40ml of ethanol with the volume percentage of 40 percent; 40ml of isopropanol with the volume percentage of 20 percent; 10ml of n-amyl alcohol with the volume percentage of 8 percent; 8-12g of settling agent; the balance being water. The settling agent is poloxamer and polyacrylamide according to the weight ratio of 1: 2 by weight ratio.
(4) And (4) centrifuging the alcohol extraction mixed solution in the step (3), and drying the obtained precipitate to obtain the galactomannan.
Example 3
The preparation method of the cassia seed-derived galactomannan of the embodiment comprises the following steps:
(1) drying semen Cassiae, and pulverizing into particles with particle diameter of 0.12mm or less to obtain coarse powder; the drying of semen Cassiae may be one of vacuum freeze drying, microwave drying, and oven drying.
(2) Dispersing the raw material coarse powder in the step (1) in 2.5L of water according to the proportion of 1kg of raw material coarse powder to obtain raw material coarse liquid;
(3) and (3) centrifuging the raw material crude liquid in the step (2), dispersing the supernatant obtained by centrifugation into the alcohol extract, uniformly stirring, and standing for 3 hours to obtain the alcohol extract. The volume ratio of the raw material crude liquid to the alcohol extract is 1: 1.
Wherein, every 100ml of the alcohol extract comprises the following components: 40ml of 38 percent ethanol by volume; 40ml of isopropanol with the volume percentage of 23 percent; 10ml of n-pentanol with the volume percentage of 5 percent; 10g of settling agent; the balance being water. The settling agent is poloxamer and polyacrylamide according to the weight ratio of 1: 10 by weight ratio.
(4) And (4) centrifuging the alcohol extraction mixed solution in the step (3), and drying the obtained precipitate to obtain the galactomannan.
Example 4
The preparation method of the cassia seed-derived galactomannan of the embodiment comprises the following steps:
(1) drying semen Cassiae, and pulverizing into particles with particle diameter of 0.12mm or less to obtain coarse powder; the drying of semen Cassiae may be one of vacuum freeze drying, microwave drying, and oven drying.
(2) Dispersing the raw material coarse powder in the step (1) in 2.5L of water according to the proportion of 1kg of raw material coarse powder to obtain raw material coarse liquid;
(3) and (3) centrifuging the raw material crude liquid in the step (2), dispersing the supernatant obtained by centrifugation into the alcohol extract, uniformly stirring, and standing for 3 hours to obtain the alcohol extract. The volume ratio of the raw material crude liquid to the alcohol extract is 1: 1.
Wherein, every 100ml of the alcohol extract comprises the following components: 40ml of 38 percent ethanol by volume; 40ml of isopropanol with the volume percentage of 23 percent; 10ml of 7% by volume n-pentanol; 10g of settling agent; the balance being water. The settling agent is poloxamer and polyacrylamide according to the weight ratio of 1: 6 by weight ratio.
(4) And (4) centrifuging the alcohol extraction mixed solution in the step (3), and drying the obtained precipitate to obtain the galactomannan.
Comparative example 1
The method for preparing the cassia seed-derived galactomannan of the comparative example is completely the same as that of example 4, and the differences are only that: in the step (3), n-pentanol is not included per 100ml of the alcohol extract.
Comparative example 2
The preparation method of the cassia seed-derived galactomannan of the comparative example is completely the same as that of the example 4, and the difference is only that: in the step (3), n-pentanol is not included and isopropanol is 35% by volume per 100ml of the alcohol extract.
Comparative example 3
The method for preparing the cassia seed-derived galactomannan of the comparative example is completely the same as that of example 4, and the differences are only that: in the step (3), the precipitation assisting agent is not included in every 100ml of the alcohol extract.
Comparative example 4
The preparation method of the cassia seed-derived galactomannan of the comparative example is completely the same as that of the example 4, and the difference is only that: in the step (3), the precipitation aid does not include poloxamer in each 100ml of the alcohol extract.
Comparative example 5
The preparation method of the cassia seed-derived galactomannan of the comparative example is completely the same as that of the example 4, and the difference is only that: in the step (3), the precipitation aid does not comprise polyacrylamide in every 100ml of the alcohol extract.
Comparative example 6
The preparation method of the cassia seed-derived galactomannan of the comparative example is completely the same as that of the example 4, and the difference is only that: in the step (3), in each 100ml of the alcohol extract, the precipitation aid is poloxamer and polyacrylamide according to the ratio of 1:1 by weight ratio.
Comparative example 7
The method for preparing the cassia seed-derived galactomannan of the comparative example is completely the same as that of example 4, and the differences are only that: in the step (3), in every 100ml of the alcohol extract, the precipitation aid is poloxamer and polyacrylamide according to the weight ratio of 1: 20 by weight ratio.
Comparative example of Effect
In order to verify the technical effect of the preparation method of the cassia seed derived galactomannan, the following tests were carried out:
the weight of the galactomannan product prepared in examples 1 to 4 and comparative examples 1 to 7 was weighed to calculate the yield of the galactomannan product in the raw meal of the endosperm of the cassia seed. The galactomannan products prepared in examples 1-4 and comparative examples 1-7 were subjected to content detection, and product purity was calculated.
The results of the above experiment are as follows:
therefore, the preparation method of the semen cassiae-derived galactomannan has high product yield and product purity.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.
Claims (6)
1. A preparation method of semen cassiae-derived galactomannan is characterized by comprising the following steps:
(1) drying semen Cassiae, and pulverizing to obtain coarse powder;
(2) dispersing the raw material coarse powder in the step (1) in water to obtain raw material coarse liquid;
(3) centrifuging the raw material crude liquid in the step (2), and dispersing the supernatant obtained by centrifugation into an alcohol extract to obtain an alcohol extract mixture;
(4) centrifuging the alcohol extraction mixed solution in the step (3) to obtain a precipitate, namely galactomannan;
in the step (3), each 100ml of the alcohol extract comprises the following components:
40ml of 38 percent ethanol by volume;
40ml of isopropanol with the volume percentage of 23 percent;
10ml of n-amyl alcohol with the volume percentage of 7 percent;
10g of settling agent;
the balance of water;
the settling agent is poloxamer and polyacrylamide according to the weight ratio of 1: 6 by weight ratio.
2. The method for producing a cassia seed-derived galactomannan according to claim 1, wherein the cassia seed is pulverized in the step (1) into particles having a particle size of 0.12mm or less.
3. The method for preparing galactomannan derived from cassia seed according to claim 1, wherein the drying of cassia seed in step (1) is one of vacuum freeze drying, microwave drying, and oven drying.
4. The method of producing a cassia seed-derived galactomannan according to claim 1, wherein in the step (2), the raw material meal is dispersed in 2 to 3L of water per 1kg of the raw material meal.
5. The method for producing a cassia seed-derived galactomannan according to claim 1, wherein the step (3) is specifically as follows: and (3) centrifuging the raw material crude liquid in the step (2), dispersing the supernatant obtained by centrifugation into the alcohol extract, uniformly stirring, and standing for 1-3h to obtain the alcohol extract.
6. The method for producing a galactomannan derived from cassia seed according to claim 1, wherein in the step (3), the volume ratio of the raw material crude liquid to the alcohol extract is 1: 1.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607997A (en) * | 2009-07-22 | 2009-12-23 | 广州城市职业学院 | The extracting method of study of semen cassia polysaccharide compound |
| CN104945527A (en) * | 2015-07-03 | 2015-09-30 | 丹娜（天津）生物科技有限公司 | Galactomannan antigen and preparation method thereof |
| CN111603500A (en) * | 2020-06-30 | 2020-09-01 | 河南中大恒源生物科技股份有限公司 | Semen cassiae extract and process technology for comprehensively developing and utilizing semen cassiae |
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- 2020-12-24 CN CN202011555774.2A patent/CN112759666B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607997A (en) * | 2009-07-22 | 2009-12-23 | 广州城市职业学院 | The extracting method of study of semen cassia polysaccharide compound |
| CN104945527A (en) * | 2015-07-03 | 2015-09-30 | 丹娜（天津）生物科技有限公司 | Galactomannan antigen and preparation method thereof |
| CN111603500A (en) * | 2020-06-30 | 2020-09-01 | 河南中大恒源生物科技股份有限公司 | Semen cassiae extract and process technology for comprehensively developing and utilizing semen cassiae |
Non-Patent Citations (3)
| Title |
|---|
| Extraction and solution properties of the galactomannan from the seeds of Cassia javanica L.;E.G.Azero;《Polymer Bulletin》;19971231;第39卷;第621-625页 * |
| Structure of a galactomannan from the seeds of Cassia angustifolia Vahl;Manjoosha等;《Carbohydrate Research》;20011231;第332卷;第439-444页 * |
| 决明子多糖结构和生物活性功能研究进展;刘金金等;《食品研究与开发》;20191210;第40卷(第23期);第212-224页 * |
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