CN107602632B - Extract of fructo-oligosaccharide and its extraction method - Google Patents
Extract of fructo-oligosaccharide and its extraction method Download PDFInfo
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Abstract
The invention relates to the technical field of fructo-oligosaccharide extraction, in particular to a thorn fructo-oligosaccharide extract and an extraction method thereof, wherein the thorn fructo-oligosaccharide extract is obtained by the following method: firstly, adding the acanthose powder into water for extraction to obtain an extracting solution; step two, filtering and evaporating the extracting solution in sequence to obtain concentrated solution; and step three, freeze-drying the concentrated solution to obtain the spinosyn fructo-oligosaccharide extract. When the extraction method of the extract of the spinosa fructo-oligosaccharide provided by the invention is used for extracting the fructo-oligosaccharide in the spinosa, the yield of the fructo-oligosaccharide reaches 23.4-27.0%, and the yield is obviously higher than that of the fructo-oligosaccharide extracted by the existing extraction method.
Description
Technical Field
The invention relates to the technical field of fructo-oligosaccharide extraction, and discloses a spinosyn fructo-oligosaccharide extract and an extraction method thereof.
Background
The spiny sugar (Alhagi-honey) is derived from dried leaf, flower, seed, whole plant and stem and leaf secretion of Asparsifolia (Asparsifolia shape) of Pegani Harmala of Leguminosae, and is in the form of small spherical granule, yellowish white, viscous, and sweet. It is a common herb used in Xinjiang folks for treating nervous headache, and is used for nourishing and strengthening body, balancing body fluid, relaxing bowel and regulating endocrine, and Uygur medicine is used for treating diseases such as dysentery, diarrhea, gastral cavity distending pain, hematuria, etc. by combining with other medicinal materials. The product also has effects in replenishing vital essence, supporting yang, astringing intestine, relieving pain, eliminating phlegm, and relieving cough.
The main components of the thorn sugar are polysaccharide and fructo-oligosaccharide. The main components of the fructo-oligosaccharide are kestose, nystose and kestose, and the fructo-oligosaccharide is the only functional oligosaccharide which has double physiological characteristics of super-strong bifidus factors and water-soluble dietary fibers.
The fructo-oligosaccharide is used as an excellent water-soluble fiber and has the functions of activating bifidobacteria, regulating the balance of intestinal flora, relaxing bowel, regulating blood fat and cholesterol, reducing blood sugar, enhancing the immunity of organisms and the like and maintaining the health of human bodies. Most of fructo-oligosaccharides are synthesized by an enzyme method, natural extracts are few, the cost is high, and simultaneously, the extraction rate is low, so that the waste of natural medicine resources is easily caused. At present, few reports about methods for extracting fructo-oligosaccharide from acanthose spurns exist, and the research on separation and purification structure and hypoglycemic effect of acanthose spurns polysaccharide (Zhengjie, Xinjiang medical university, 2016) discloses that fructo-oligosaccharide in acanthose spurns is extracted by an ultrasonic extraction method, but the yield (extraction rate) of fructo-oligosaccharide is low.
Disclosure of Invention
The invention provides a spinosyn fructo-oligosaccharide extract and an extraction method thereof, overcomes the defects of the prior art, and can effectively solve the problem of low extraction rate of fructo-oligosaccharide in the existing extraction method of the spinosyn fructo-oligosaccharide extract.
One of the technical schemes of the invention is realized by the following measures: a polysaccharide fructo-oligosaccharide extract is prepared by the following steps: firstly, adding the thorn sugar powder into water according to the material-liquid ratio of 1: 30-40 g/ml for extraction for 2-3 hours to obtain an extracting solution, wherein the extraction temperature is 90-95 ℃; secondly, filtering and evaporating the extracting solution in sequence to obtain concentrated solution, wherein the temperature of evaporation concentration is 60-65 ℃, and the filtered extracting solution is evaporated and concentrated to 1/9-1/8 of the volume before evaporation concentration to obtain concentrated solution; and step three, freeze-drying the concentrated solution to obtain the spinosyn fructo-oligosaccharide extract.
The following is a further optimization or/and improvement of one of the above-mentioned technical solutions of the invention:
the freeze drying temperature is-50 deg.C to-30 deg.C, and freeze drying the concentrated solution to obtain fructo-oligosaccharide extract; or/and the grain size of the acanthopanax senticosus powder material is required to be as follows: 0mm < the grain size of the acanthose powder material <0.250 mm.
In the first step, the thorn sugar is crushed to obtain the thorn sugar powder.
The filtration is performed by suction filtration.
The water is distilled water.
The second technical scheme of the invention is realized by the following measures: a method for extracting a spinosyn fructo-oligosaccharide extract comprises the following steps: firstly, adding the thorn sugar powder into water according to the material-liquid ratio of 1: 30-40 g/ml for extraction for 2-3 hours to obtain an extracting solution, wherein the extraction temperature is 90-95 ℃; secondly, filtering and evaporating the extracting solution in sequence to obtain concentrated solution, wherein the temperature of evaporation concentration is 60-65 ℃, and the filtered extracting solution is evaporated and concentrated to 1/9-1/8 of the volume before evaporation concentration to obtain concentrated solution; and step three, freeze-drying the concentrated solution to obtain the spinosyn fructo-oligosaccharide extract.
The following is further optimization or/and improvement of the second technical scheme of the invention:
the freeze drying temperature is-50 deg.C to-30 deg.C, and freeze drying the concentrated solution to obtain fructo-oligosaccharide extract; or/and the grain size of the acanthopanax senticosus powder material is required to be as follows: 0mm < the grain size of the acanthose powder material <0.250 mm.
In the first step, the thorn sugar is crushed to obtain the thorn sugar powder.
The filtration is performed by suction filtration.
The water is distilled water.
When the extraction method of the extract of the spinosa fructo-oligosaccharide provided by the invention is used for extracting the fructo-oligosaccharide in the spinosa, the yield of the fructo-oligosaccharide reaches 23.4-27.0%, and the yield is obviously higher than that of the fructo-oligosaccharide extracted by the existing extraction method.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments may be determined according to the technical solutions and practical situations of the present invention. The various chemical reagents and chemical articles mentioned in the invention are all the chemical reagents and chemical articles which are well known and commonly used in the prior art, unless otherwise specified; the normal temperature and room temperature in the present invention generally mean a temperature of 15 ℃ to 25 ℃, and are generally defined as 25 ℃.
The invention is further described below with reference to the following examples:
example 1: the extract of the spinosyn fructo-oligosaccharide is obtained by the following extraction method: firstly, adding the thorn sugar powder into water according to the material-liquid ratio of 1: 30-40 g/ml for extraction for 2-3 hours to obtain an extracting solution, wherein the extraction temperature is 90-95 ℃; secondly, filtering and evaporating the extracting solution in sequence to obtain concentrated solution, wherein the temperature of evaporation concentration is 60-65 ℃, and the filtered extracting solution is evaporated and concentrated to 1/9-1/8 of the volume before evaporation concentration to obtain concentrated solution; and step three, freeze-drying the concentrated solution to obtain the spinosyn fructo-oligosaccharide extract.
According to the extraction method of the embodiment, the extraction rate (yield) of the fructo-oligosaccharide reaches 23.4 percent to 27.0 percent. When the existing extraction method of the fructo-oligosaccharide (separation and purification structure analysis of the polysaccharide of the spinosad and research on the effect of reducing blood sugar, Zhengjie, Xinjiang medical university, 2016) is adopted to extract the fructo-oligosaccharide, the yield of the fructo-oligosaccharide reaches 21.2 percent to the maximum. Therefore, the extraction method described in this example can improve the yield of fructo-oligosaccharide in the spinosad.
Moreover, the extraction method described in the embodiment is simple to operate, has mild extraction conditions, has low requirements on extraction equipment, is easy to industrialize, does not damage active ingredients, and has no organic solvent residue.
Yield (percentage content) = (m)1/m2）×100%,m1M is the mass of the spinosyn fructo-oligosaccharide2The mass of the thorn sugar.
Example 2: the extract of the spinosyn fructo-oligosaccharide is obtained by the following extraction method: firstly, adding the thorn sugar powder into water according to the material-liquid ratio of 1:30 or 40 g/ml for extraction for 2 hours or 3 hours to obtain an extracting solution, wherein the extraction temperature is 90 ℃ or 95 ℃; secondly, filtering and evaporating the extracting solution in sequence to obtain concentrated solution, wherein the temperature of evaporation concentration is 60 ℃ or 65 ℃, and the filtered extracting solution is evaporated and concentrated to 1/9 or 1/8 of the volume before evaporation concentration to obtain concentrated solution; and step three, freeze-drying the concentrated solution to obtain the spinosyn fructo-oligosaccharide extract.
Example 3: as optimization of the above embodiment, the temperature of freeze drying is-50 deg.C to-30 deg.C, and the concentrated solution is freeze dried to fluffy state to obtain fructo-oligosaccharide extract; or/and the grain size of the acanthopanax senticosus powder material is required to be as follows: 0mm < the grain size of the acanthose powder material <0.250 mm.
Example 4: as an optimization of the above embodiment, in the first step, the acanthose powder is obtained by pulverizing the acanthose.
Example 5: as optimization of the above example, suction filtration was used for filtration.
Example 6: as a preferred embodiment, the water is distilled water.
When distilled water is adopted for extraction, the introduction of impurity ions can be avoided, and the purity of the spinosyn fructo-oligosaccharide extract is ensured.
Example 7: the extract of the spinosyn fructo-oligosaccharide is obtained by the following extraction method: firstly, adding the thorn sugar powder into water according to the material-liquid ratio of 1:30g/ml for extraction for 2 hours to obtain an extracting solution, wherein the extraction temperature is 90 ℃; secondly, filtering and evaporating the extracting solution in sequence to obtain concentrated solution, wherein the temperature of evaporation concentration is 60-65 ℃, and the filtered extracting solution is evaporated and concentrated to 1/8 of the volume before evaporation concentration to obtain concentrated solution; and step three, freeze-drying the concentrated solution to obtain the spinosyn fructo-oligosaccharide extract.
According to the extract of the spinosyn fructo-oligosaccharide obtained in the embodiment, the yield of the fructo-oligosaccharide reaches 25.0 percent.
Example 8: the extract of the spinosyn fructo-oligosaccharide is obtained by the following extraction method: firstly, adding the thorn sugar powder into water according to the material-liquid ratio of 1:30g/ml for extraction for 2 hours to obtain an extracting solution, wherein the extraction temperature is 92 ℃; secondly, filtering and evaporating the extracting solution in sequence to obtain concentrated solution, wherein the temperature of evaporation concentration is 60-65 ℃, and the filtered extracting solution is evaporated and concentrated to 1/8 of the volume before evaporation concentration to obtain concentrated solution; and step three, freeze-drying the concentrated solution to obtain the spinosyn fructo-oligosaccharide extract.
According to the extract of the spinosyn fructo-oligosaccharide obtained in the embodiment, the yield of the fructo-oligosaccharide reaches 27.0 percent.
Example 9: the extract of the spinosyn fructo-oligosaccharide is obtained by the following extraction method: firstly, adding the thorn sugar powder into water according to the material-liquid ratio of 1:30g/ml for extraction for 2 hours to obtain an extracting solution, wherein the extraction temperature is 95 ℃; secondly, filtering and evaporating the extracting solution in sequence to obtain concentrated solution, wherein the temperature of evaporation concentration is 60-65 ℃, and the filtered extracting solution is evaporated and concentrated to 1/8 of the volume before evaporation concentration to obtain concentrated solution; and step three, freeze-drying the concentrated solution to obtain the spinosyn fructo-oligosaccharide extract.
According to the extract of the spinosyn fructo-oligosaccharide obtained in the embodiment, the yield of the fructo-oligosaccharide reaches 24.7 percent.
Example 10: the extract of the spinosyn fructo-oligosaccharide is obtained by the following extraction method: firstly, adding the thorn sugar powder into water according to the material-liquid ratio of 1:40 g/ml for extraction for 3 hours to obtain an extracting solution, wherein the extraction temperature is 92 ℃; secondly, filtering and evaporating the extracting solution in sequence to obtain concentrated solution, wherein the temperature of evaporation concentration is 60-65 ℃, and the filtered extracting solution is evaporated and concentrated to 1/9 of the volume before evaporation concentration to obtain concentrated solution; and step three, freeze-drying the concentrated solution to obtain the spinosyn fructo-oligosaccharide extract.
According to the extract of the spinosyn fructo-oligosaccharide obtained in the embodiment, the yield of the fructo-oligosaccharide reaches 23.7 percent.
Example 11: the extract of the spinosyn fructo-oligosaccharide is obtained by the following extraction method: firstly, adding the thorn sugar powder into water according to the material-liquid ratio of 1:40 g/ml for extraction for 2 hours to obtain an extracting solution, wherein the extraction temperature is 95 ℃; secondly, filtering and evaporating the extracting solution in sequence to obtain concentrated solution, wherein the temperature of evaporation concentration is 60-65 ℃, and the filtered extracting solution is evaporated and concentrated to 1/8 of the volume before evaporation concentration to obtain concentrated solution; and step three, freeze-drying the concentrated solution to obtain the spinosyn fructo-oligosaccharide extract.
According to the extract of the spinosyn fructo-oligosaccharide obtained in the embodiment, the yield of the fructo-oligosaccharide reaches 23.4 percent.
When the extraction method of the present invention is used to extract fructo-oligosaccharide from the thorn sugar, the feed-liquid ratio, the extraction time and the extraction temperature have a great influence on the yield of the fructo-oligosaccharide, and the following comparative examples are provided.
Extraction time
Comparative example 1: 5g of the spinosad was weighed and extracted for 1 hour, and other extraction parameters were the same as those in example 11.
The extract obtained by the extraction method of the comparative example has the yield of the fructo-oligosaccharide of 17 percent.
Comparative example 2: 5g of the spinosad was weighed and extracted for 1.5 hours, and other extraction parameters were the same as those in example 11.
The extract obtained by the extraction method of the comparative example has the yield of fructo-oligosaccharide of 16 percent.
Comparative example 3: 5g of the spinosad was weighed and extracted for 3.5 hours, and other extraction parameters were the same as those in example 11.
The extract obtained by the extraction method of the comparative example has the yield of fructo-oligosaccharide of 14.5 percent.
It can be seen from comparative examples 1 to 3 that the yield of fructooligosaccharides is much less than the yield of fructooligosaccharides obtained by the method of the present invention as described in the above examples, when the extraction time described in comparative examples 1 to 3 is used.
Temperature of extraction
Comparative example 4: weighing 5g of acanthose, extracting at 75 deg.C, and performing the same extraction with the same extraction parameters as in example 11.
The extract obtained in this comparative example showed a fructooligosaccharide yield of 14.5%.
Comparative example 5: weighing 5g of acanthose, extracting at 80 deg.C, and performing the same extraction with the same extraction parameters as in example 11.
The extract obtained in this comparative example showed an oligofructose yield of 18.0%.
Comparative example 6: weighing 5g of acanthose, extracting at 85 deg.C, and performing the same extraction with the same extraction parameters as in example 11.
The extract obtained in this comparative example showed a fructooligosaccharide yield of 16.3%.
Comparative example 7: weighing 5g of acanthose, extracting at 100 deg.C, and performing the same extraction with the same extraction parameters as in example 11.
The extract obtained in this comparative example showed a fructooligosaccharide yield of 17.2%.
It can be seen from comparative examples 4 to 7 that the yield of fructooligosaccharides using the extraction temperatures described in comparative examples 4 to 7 is much less than the yield of fructooligosaccharides using the process of the invention described in the above example.
In conclusion, when the extraction method of the extract of the spinosa fructo-oligosaccharide is used for extracting the fructo-oligosaccharide in the spinosa, the yield of the fructo-oligosaccharide reaches 23.4-27.0 percent, which is obviously higher than the yield of the extraction of the fructo-oligosaccharide by the existing extraction method, and moreover, the extraction method of the extract of the fructo-oligosaccharide of the spinosa fructo-oligosaccharide is simple to operate, has low requirement on extraction equipment, is easy to industrialize, and does not damage active ingredients (polysaccharide and fructo-oligosaccharide) and has no organic solvent residue.
The technical characteristics form an embodiment of the invention, which has strong adaptability and implementation effect, and unnecessary technical characteristics can be increased or decreased according to actual needs to meet the requirements of different situations.
Claims (8)
1. The extraction method of the spinosyn fructo-oligosaccharide extract is characterized by comprising the following steps: firstly, adding the thorn sugar powder into water according to the material-liquid ratio of 1: 30-40 g/ml for extraction for 2-3 hours to obtain an extracting solution, wherein the extraction temperature is 90-95 ℃; secondly, filtering and evaporating the extracting solution in sequence to obtain concentrated solution, wherein the temperature of evaporation concentration is 60-65 ℃, and the filtered extracting solution is evaporated and concentrated to 1/9-1/8 of the volume before evaporation concentration to obtain concentrated solution; and step three, freeze-drying the concentrated solution to obtain the spinosyn fructo-oligosaccharide extract.
2. The method for extracting fructo-oligosaccharide extract according to claim 1, wherein the temperature of freeze-drying is from-50 ℃ to-30 ℃, and the concentrated solution is freeze-dried to be fluffy to obtain fructo-oligosaccharide extract; or/and the grain size of the acanthopanax senticosus powder material is required to be as follows: 0mm < the grain size of the acanthose powder material <0.250 mm.
3. The method for extracting a fructo-oligosaccharide extract with a thorn according to claim 1 or 2, characterized in that in the first step, the thorn is pulverized to obtain a thorn powder.
4. The method for extracting fructo-oligosaccharide extract with spiny sugar as claimed in claim 1 or 2, wherein the filtration is performed by suction filtration.
5. The method for extracting fructo-oligosaccharide extract according to claim 3, wherein the filtration is performed by suction filtration.
6. The method for extracting fructo-oligosaccharide extract with sugar as claimed in claim 1, 2 or 5, wherein the water is distilled water.
7. The method for extracting fructo-oligosaccharide extract with spiny sugar as claimed in claim 3, wherein the water is distilled water.
8. The method for extracting fructo-oligosaccharide extract with spiny sugar as claimed in claim 4, wherein the water is distilled water.
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