CN113373190B - Method for preparing galactomannan from semen Trigonellae - Google Patents

Method for preparing galactomannan from semen Trigonellae Download PDF

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CN113373190B
CN113373190B CN202110582035.0A CN202110582035A CN113373190B CN 113373190 B CN113373190 B CN 113373190B CN 202110582035 A CN202110582035 A CN 202110582035A CN 113373190 B CN113373190 B CN 113373190B
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galactomannan
fenugreek
semen trigonellae
mixture
preparing
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CN113373190A (en
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张伟
曹毅
武建
刘燕静
袁江宏
袁润
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Chengde Kangerrun Food Co ltd
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    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/04Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
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    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/14Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase

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Abstract

The invention discloses a method for preparing galactomannan from fenugreek. The method comprises the steps of firstly peeling fenugreek and lima beans, then adding water for tempering, mixing and crushing; then sanding the mixture in a sanding machine; adding water, mixing well to obtain water solution, adding mannase and galactosidase, and hydrolyzing to obtain enzymatic hydrolysate; finally, inactivating the enzymolysis liquid, cooling to room temperature, filtering, decolorizing, concentrating to obtain syrup, and vacuum drying to obtain galactomannan. The invention adopts fenugreek and lima beans as extraction raw materials to prepare the galactomannan, compared with the galactomannan obtained by singly adopting the fenugreek, the galactomannan has better solubility and higher viscosity, and part of the galactomannan is decomposed into mannan-oligosaccharide by adopting the micro-fermentation of mannase and galactosidase, so that the prepared galactomannan is easier to be absorbed and utilized by human bodies.

Description

Method for preparing galactomannan from semen Trigonellae
Technical Field
The invention belongs to the technical field of natural food additives, and particularly relates to a method for preparing galactomannan from fenugreek.
Background
Galactomannan is a polysaccharide comprising mannose backbones and galactose side groups, which is a polysaccharide having linear (1-4) -linked β -D mannose backbones linked at their 6-linkage points to α -D galactose, i.e. 1-6-linked α -D galactopyranoses. The galactomannans are derived from fenugreek gum, guar gum, carob gum and tara gum, and the galactomannans of different plant origin have different degrees of branching.
Trigonella foenum-graecum L, a commonly known name for Trigonella foenum-graecum L, a plant of Trigonella of Leguminosae. Annual herbaceous plant with height of 30-80 cm, developed root system, upright stem, three pinnate branchesLeaf and petiole are flat, flowering period is 4-7 months, and fruit period is 7-9 months. Fenugreek can be used as a raw material for preparing galactomannan, and patent 02138257.3 discloses a production method of fast-dispersing and instant galactomannan gum. It is made up by using high-quality industrial-grade galactomannan film (trigonella film) as raw material through the processes of hydration, drying, pulverizing, grading, edible alcohol soaking treatment, centrifugal desolventizing and vacuum drying. The total dissolution time of the prepared galactomannan gum is 25min, the viscosity of 1% gum solution reaches 350mPa.s (170 s) -1 ) Although the dissolution properties are improved compared to galactomannan gums from other plant species, the requirements for rapid dissolution and improved viscosity are still not met.
Disclosure of Invention
The invention aims to provide a method for preparing galactomannan from fenugreek.
A method for preparing galactomannan from semen Trigonellae comprises the following steps:
(1) Peeling semen Trigonellae and semen Trigonellae, and adding 2-4% water for tempering for 6-12min;
(2) Mixing the peeled and modified fenugreek and lima beans, crushing, and sieving by a sieve of 20-30 meshes; then sanding the mixture in a sand mill, and sieving the mixture by a sieve with 50 to 80 meshes;
(3) Adding water with the mass 3-10 times of the material in the step (2), uniformly mixing to prepare an aqueous solution, adding mannase and galactosidase, and hydrolyzing to prepare an enzymatic hydrolysate;
(4) Inactivating the enzymolysis liquid prepared in the step (3) in a boiling water bath, cooling to room temperature, filtering, decolorizing and concentrating to obtain syrup;
(5) And (5) drying the syrup prepared in the step (4) in vacuum to obtain the galactomannan.
The usage amount mass ratio of the fenugreek to the lima beans is (2-5): 1.
the addition amount of the mannase is 100-200U per gram of the mixed material in the step (2).
The addition amount of the galactosidase is 50-100U per gram of the mixed material in the step (2).
The hydrolysis temperature in the step (3) is 30-50 ℃, and the hydrolysis time is 1-5h.
And the decolorization adopts activated carbon for decolorization.
The temperature of the vacuum drying is 55-75 ℃, and the vacuum degree is 0.05-0.1MPa.
The invention has the beneficial effects that: the invention adopts fenugreek and lima beans as extraction raw materials to prepare the galactomannan, compared with the galactomannan obtained by singly adopting the fenugreek, the galactomannan has better solubility and higher viscosity, and part of the galactomannan is decomposed into mannan-oligosaccharide by adopting the micro-fermentation of mannase and galactosidase, so that the prepared galactomannan is easier to be absorbed and utilized by human bodies.
Drawings
FIG. 1 shows the time for a sample to dissolve in water to reach maximum viscosity after co-extraction of fenugreek with other plant seeds.
FIG. 2 is a graph showing the viscosity of the samples after co-extraction of fenugreek with other plant seeds.
Figure 3 is the time for the sample to dissolve in water to reach maximum viscosity after different mass ratios of fenugreek and lima beans were co-extracted.
Figure 4 is the viscosity of the samples after co-extraction of different mass ratios of fenugreek and lima beans.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following more detailed description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Example 1
A method for preparing galactomannan from semen Trigonellae comprises the following steps:
(1) Peeling semen Trigonellae, and adding 3% water for tempering for 10min;
(2) Crushing the peeled and tempered fenugreek, and sieving the crushed fenugreek with a 25-mesh sieve; then sanding the mixture in a sand mill, and sieving the mixture by a 60-mesh sieve;
(3) Adding water with the mass 5 times that of the material in the step (2), uniformly mixing to prepare an aqueous solution, adding mannase and galactosidase, and hydrolyzing to prepare an enzymatic hydrolysate; the addition amount of the mannanase is 150U per gram of the mixed material in the step (2); the addition amount of the galactosidase is 80U per gram of the mixed material in the step (2); the hydrolysis temperature is 45 ℃, and the hydrolysis time is 3h;
(4) Inactivating the enzymolysis liquid prepared in the step (3) in a boiling water bath, cooling to room temperature, filtering, decoloring with active carbon, and concentrating to obtain syrup;
(5) Vacuum drying the syrup prepared in the step (4) to obtain galactomannan; the temperature of the vacuum drying is 60 ℃, and the vacuum degree is 0.08MPa.
Preparing a 1% concentration sample solution; measuring the time for the sample to be dissolved in water to reach the maximum viscosity, wherein the standard for reaching the maximum viscosity is that the solution is seen to be a uniform solution visually, no bubbles or lumps exist, the glass rod has resistance feeling when being stirred, and the glass rod is adhered to the sample after being picked up and does not fall within 5 s; measuring the time for dissolution to reach the maximum viscosity to be 38min; the viscosity was measured to be 352mPa.s (170 s) using a capillary viscometer -1 )。
Example 2
To increase the viscosity of the galactomannan and at the same time reduce the time to reach maximum viscosity upon dissolution in water, the inventors tried co-extraction with fenugreek with other galactomannan-containing plant seeds in a mass ratio of 1:1, the experimental method is the same as that of the embodiment 1, and the selected plants comprise ormosia, cassia seed, gelia, lima bean, pepper and sesame, pig dung bean, winged podocarpus and sesbania; a1% strength sample solution was prepared, and the time until the sample dissolved in water to reach the maximum viscosity and the viscosity were measured, and the measurement results are shown in FIGS. 1 and 2.
As can be seen from fig. 1 and 2, the time for the sample extracted from fenugreek and fenugreek to reach the maximum viscosity is the shortest and the viscosity is the maximum.
Example 3 extraction ratio optimization
Selecting fenugreek and fenugreek beans as co-extraction raw materials, exploring the optimal dosage ratio of the fenugreek and the fenugreek beans, and setting the dosage mass ratio of the fenugreek and the fenugreek beans as 1: 3. 1: 2. 1: 1. 2: 1. 3: 1. 4: 1. 5: 1. 6:1, the experimental method is the same as example 1; after the extraction operation was completed, a 1% strength sample solution was prepared, and the time until the sample dissolved in water to reach the maximum viscosity and the viscosity were measured, and the results are shown in fig. 3 and 4.
As can be seen from fig. 3 and 4, the mass ratio of fenugreek to fenugreek is 3:1, the time for the sample to dissolve in water to reach the maximum viscosity is shortest, and the viscosity is maximum.
Example 4
A method for preparing galactomannan from semen Trigonellae comprises the following steps:
(1) Peeling semen Trigonellae and semen Trigonellae, and adding 3% water for tempering for 10min;
(2) Respectively crushing the peeled and tempered fenugreek and lima beans according to the mass ratio of 3:1, uniformly mixing, and sieving by a 25-mesh sieve; then sanding the mixture in a sand mill, and sieving the mixture by a 60-mesh sieve;
(3) Adding water with the mass 5 times of that of the material in the step (2), uniformly mixing to prepare an aqueous solution, adding mannase and galactosidase, and hydrolyzing to prepare an enzymatic hydrolysate; the addition amount of the mannanase is 150U per gram of the mixed material in the step (2); the addition amount of the galactosidase is 80U per gram of the mixed material in the step (2); the hydrolysis temperature is 45 ℃, and the hydrolysis time is 3h;
(4) Inactivating the enzymolysis liquid prepared in the step (3) in a boiling water bath, cooling to room temperature, filtering, decoloring with active carbon, and concentrating to obtain syrup;
(5) Vacuum drying the syrup prepared in the step (4) to obtain galactomannan; the temperature of the vacuum drying is 60 ℃, and the vacuum degree is 0.08MPa.
Example 5
A method for preparing galactomannan from semen Trigonellae comprises the following steps:
(1) Peeling semen Trigonellae and semen Trigonellae, and adding 3% water for tempering for 10min;
(2) Respectively crushing the peeled and tempered fenugreek and lima beans, and mixing the crushed materials according to a mass ratio of 4:1, uniformly mixing, and sieving by a 25-mesh sieve; then sanding the mixture in a sand mill, and sieving the mixture by a 60-mesh sieve;
(3) Adding water with the mass 6 times of that of the material in the step (2), uniformly mixing to prepare an aqueous solution, adding mannase and galactosidase, and hydrolyzing to prepare an enzymatic hydrolysate; the addition amount of the mannanase is 200U per gram of the mixed material in the step (2); the addition amount of the galactosidase is 100U per gram of the mixed material in the step (2); the hydrolysis temperature is 40 ℃, and the hydrolysis time is 3h;
(4) Inactivating the enzymolysis liquid prepared in the step (3) in a boiling water bath, cooling to room temperature, filtering, decoloring with active carbon, and concentrating to obtain syrup;
(5) Vacuum drying the syrup prepared in the step (4) to obtain galactomannan; the temperature of the vacuum drying is 60 ℃, and the vacuum degree is 0.06MPa.
Example 6
A method for preparing galactomannan from semen Trigonellae comprises the following steps:
(1) Peeling semen Trigonellae and semen Trigonellae, and adding 3% water for tempering for 10min;
(2) Respectively crushing the peeled and tempered fenugreek and lima beans according to a mass ratio of 2:1, uniformly mixing, and sieving by a 25-mesh sieve; then sanding the mixture in a sand mill, and sieving the mixture by a 60-mesh sieve;
(3) Adding water with the mass 4 times that of the material in the step (2), uniformly mixing to prepare an aqueous solution, adding mannase and galactosidase, and hydrolyzing to prepare an enzymatic hydrolysate; the addition amount of the mannanase is 100U per gram of the mixed material in the step (2); the addition amount of the galactosidase is 60U per gram of the mixed material in the step (2); the hydrolysis temperature is 50 ℃, and the hydrolysis time is 2h;
(4) Inactivating the enzymolysis liquid prepared in the step (3) in a boiling water bath, cooling to room temperature, filtering, decoloring with active carbon, and concentrating to obtain syrup;
(5) Vacuum drying the syrup prepared in the step (4) to obtain galactomannan; the temperature of the vacuum drying is 60 ℃, and the vacuum degree is 0.05MPa.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (6)

1. A method for preparing galactomannan from semen Trigonellae is characterized by comprising the following steps:
(1) Peeling semen Trigonellae and semen Trigonellae, and adding 2-4% water for tempering for 6-12min;
(2) Mixing the peeled and modified fenugreek and lima beans, crushing, and sieving by a sieve of 20-30 meshes; then sanding the mixture in a sand mill, and sieving the mixture by a sieve with 50 to 80 meshes;
(3) Adding water with the mass 3-10 times of that of the material in the step (2), uniformly mixing to prepare an aqueous solution, adding mannase and galactosidase, and hydrolyzing to prepare an enzymatic hydrolysate;
(4) Inactivating the enzymolysis liquid prepared in the step (3) in a boiling water bath, cooling to room temperature, filtering, decolorizing and concentrating to obtain syrup;
(5) Vacuum drying the syrup prepared in the step (4) to obtain galactomannan;
the usage amount mass ratio of the fenugreek to the lima beans is (2-5): 1.
2. the method for preparing galactomannan from semen Trigonellae according to claim 1, wherein the mannanase is added in an amount of 100-200U per gram of the mixture of step (2).
3. The method for preparing galactomannan from semen Trigonellae as claimed in claim 1, wherein the amount of galactosidase added is 50-100U per gram of the mixture of step (2).
4. The method for preparing galactomannan from semen Trigonellae as claimed in claim 1, wherein the hydrolysis temperature in step (3) is 30-50 deg.C, and the hydrolysis time is 1-5h.
5. The method of producing galactomannan from semen Trigonellae as claimed in claim 1, wherein said decolorizing is with activated carbon.
6. The process for the preparation of galactomannan from semen Trigonellae as claimed in claim 1, wherein the temperature of vacuum drying is 55-75 deg.C and the vacuum is 0.05-0.1MPa.
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Citations (2)

* Cited by examiner, † Cited by third party
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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
CN112760311A (en) * 2021-01-29 2021-05-07 南京林业大学 Enzyme solution with relatively excellent enzyme activity ratio of beta-mannase to alpha-galactosidase, and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
US7338675B2 (en) * 2002-05-10 2008-03-04 Tsi Health Sciences, Inc. Fenugreek seed bio-active compositions and methods for extracting same
CA2678311A1 (en) * 2009-09-04 2011-03-04 Emerald Seed Products Ltd. Fenugreek composition for use in improving milk production in mammals

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN112760311A (en) * 2021-01-29 2021-05-07 南京林业大学 Enzyme solution with relatively excellent enzyme activity ratio of beta-mannase to alpha-galactosidase, and preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
半乳甘露聚糖种子胶的研究进展;杨永利;《西北师范大学学报》;19991231;第35卷(第1期);第104-110页 *

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