CN115109108A - Method for extracting buckwheat rutin - Google Patents
Method for extracting buckwheat rutin Download PDFInfo
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- CN115109108A CN115109108A CN202210705847.4A CN202210705847A CN115109108A CN 115109108 A CN115109108 A CN 115109108A CN 202210705847 A CN202210705847 A CN 202210705847A CN 115109108 A CN115109108 A CN 115109108A
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- Prior art keywords
- tartary buckwheat
- rutin
- extracting solution
- buckwheat
- extraction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
Abstract
The invention discloses a method for extracting buckwheat rutin, which comprises the following steps: freezing and grinding the tartary buckwheat tissues to obtain tartary buckwheat powder; under the ultrasonic condition, the tartary buckwheat powder is placed in an extracting solution with the pH value of 8.5-9.5 for extraction and filtration to obtain a tartary buckwheat extracting solution, wherein the extracting solution comprises the following components: ethanol, sodium sulfite and water; adjusting the pH value of the tartary buckwheat extracting solution to 2.5-3.5, standing and filtering to obtain a tartary buckwheat rutin crude product; washing the tartary buckwheat rutin crude product with water, and drying in vacuum to obtain the tartary buckwheat rutin; according to the extraction method, the tissues and cell walls of the tartary buckwheat can be crushed by freezing and grinding and then ultrasonic extraction, so that the precipitation of rutin in the tartary buckwheat is fully promoted, and the oxidation loss of rutin in the tartary buckwheat is reduced by adding sodium sulfite; in addition, the extraction rate of the tartary buckwheat rutin can be better improved by limiting the material-liquid ratio, the extraction temperature, the extraction time and the content of the components in the extracting solution.
Description
Technical Field
The invention relates to the technical field of extraction of buckwheat rutin, and particularly relates to an extraction method of buckwheat rutin.
Background
Fagopyrum tataricum (F. tataricum) belongs to Polygonaceae (Polygonaceae) Fagopyrum genus (Fagopyrum Mil) annual herbaceous plant. The tartary buckwheat is rich in nutrition, and the content of protein, fat, vitamins and trace elements is generally higher than that of rice, wheat and corn. The tartary buckwheat also contains special nutrients such as rutin which are not possessed by other grain crops, and has the medical functions of assisting in treating cardiovascular and cerebrovascular diseases, hypertension, diabetes, cancer, clearing heat, removing toxicity, diminishing inflammation and the like. In recent years, along with the improvement of living standard of people, the development and utilization of tartary buckwheat has raised the trend of heat in the food and medicine world in China, and the development of health foods such as tartary buckwheat tea, noodles and snacks is concerned by food processing enterprises at home and abroad.
The tartary buckwheat has the effects of reducing blood pressure, reducing blood sugar and the like, and active substances in the tartary buckwheat comprise tartary buckwheat rutin which is clinically used for the auxiliary treatment of hypertension, and the prevention and treatment of diabetes and combined hyperlipidemia; in addition, rutin can be used as natural antioxidant and pigment, and can be widely used in the fields of health food and cosmetics.
At present, rutin is generally extracted by a method of soaking raw materials, and then the raw materials are directly extracted, filtered and dried by adopting a solvent to obtain the rutin, but the yield and the purity of the rutin in the existing preparation method are lower.
Disclosure of Invention
The invention aims to provide an extraction method of buckwheat rutin, which can effectively destroy buckwheat histiocyte, fully promote precipitation of buckwheat rutin, reduce oxidation loss of buckwheat rutin and finally achieve the purpose of improving extraction rate and purity of buckwheat rutin.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a method for extracting buckwheat rutin, which comprises the following steps:
(a) freezing and grinding the tartary buckwheat tissues to obtain tartary buckwheat powder;
(b) under the ultrasonic condition, the tartary buckwheat powder is placed in an extracting solution with the pH value of 8.5-9.5 for extraction and filtration to obtain a tartary buckwheat extracting solution, wherein the extracting solution comprises the following components: ethanol, sodium sulfite and water;
(c) adjusting the pH value of the tartary buckwheat extracting solution to 2.5-3.5, standing and filtering to obtain a tartary buckwheat rutin crude product;
(d) and (3) washing the buckwheat rutin crude product with water, and drying in vacuum to obtain the buckwheat rutin.
Preferably, in the step (b), the volume concentration of the ethanol in the extracting solution is 50-70%, and the mass concentration of the sodium sulfite is 0.2-0.3%.
Preferably, in the step (b), the mass ratio of the tartary buckwheat powder to the extracting solution is 1: 8-12.
Preferably, in the step (b), the extraction temperature is room temperature, and the extraction time is 0.5-1 h.
Preferably, in the step (b), the ultrasonic power is 600-800W.
Preferably, in the step (a), the grinding time is 0.2-0.5 h.
Preferably, in the step (a), the tartary buckwheat tissue is at least one of fresh tartary buckwheat flowers, leaves and stems in the flowering period.
Preferably, in the step (c), the standing time is not less than 2 h.
Compared with the prior art, the invention has the beneficial effects that at least:
according to the extraction method, the tissues and cell walls of the tartary buckwheat can be crushed by freezing and grinding and then ultrasonic extraction, so that the precipitation of rutin in the tartary buckwheat is fully promoted, and the oxidation loss of rutin in the tartary buckwheat is reduced by adding sodium sulfite; in addition, the extraction rate of the buckwheat rutin can be better improved by limiting the material-liquid ratio, the extraction temperature, the extraction time and the component content in the extracting solution.
Detailed Description
The following describes embodiments of the present invention in detail with reference to the following embodiments. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
The embodiment of the invention provides an extraction method of tartary buckwheat rutin, which comprises the following steps:
(a) freezing and grinding the tartary buckwheat tissues to obtain tartary buckwheat powder;
(b) under the ultrasonic condition, the tartary buckwheat powder is placed in an extracting solution with the pH value of 8.5-9.5 for extraction and filtration to obtain a tartary buckwheat extracting solution, wherein the extracting solution comprises the following components: ethanol, sodium sulfite and water;
(c) adjusting the pH value of the tartary buckwheat extracting solution to 2.5-3.5, standing and filtering to obtain a tartary buckwheat rutin crude product;
(d) and (3) washing the buckwheat rutin crude product with water, and drying in vacuum to obtain the buckwheat rutin.
The extraction method comprises the steps of firstly freezing and grinding the tartary buckwheat tissues and then carrying out ultrasonic extraction, so that the tartary buckwheat tissues and tartary buckwheat cell walls can be thoroughly crushed, the precipitation of rutin is fully promoted, and meanwhile, the oxidation loss of rutin in the tartary buckwheat is effectively reduced by adding sodium sulfite; the extraction method of the invention obviously improves the extraction rate of the buckwheat rutin and the purity of the extracted product.
In one embodiment, in the step (b), the volume concentration of ethanol in the extracting solution is 50-70%, and the mass concentration of sodium sulfite is 0.2-0.3%;
the mass ratio of the tartary buckwheat powder to the extracting solution is 1: 8-12;
the extraction temperature is room temperature, and the extraction time is 0.5-1 h;
the ultrasonic power is 600-800W.
The extraction rate of the buckwheat rutin can be better improved by limiting the material-liquid ratio, the extraction temperature, the extraction time and the component content in the extracting solution.
In one embodiment, in the step (a), the grinding time is 0.2 to 0.5 h.
The Fagopyrum tataricum tissue is at least one of fresh Fagopyrum tataricum flower, leaf and stem in flowering period.
The rutin is more abundant in the flowers, leaves and stems of the tartary buckwheat in the flowering period, so that the extraction rate of the rutin can be better improved by selecting fresh tartary buckwheat tissues at a specific time, and in addition, the rutin can be separated out from the tartary buckwheat through the limitation on the grinding time.
In yet another embodiment, in step (c), the standing time is not less than 2 hours; preferably, 4 to 6 hours. For example, it may be 4h, 5h or 6 h.
The technical solution of the present invention is further described in detail by the following specific examples.
Example 1
The embodiment is a method for extracting buckwheat rutin, which comprises the following steps:
(a) selecting fresh tartary buckwheat flowers in a flowering period, and then carrying out freeze grinding on the tartary buckwheat flowers for 0.2h to obtain tartary buckwheat powder;
(b) under the ultrasonic condition of 600W, according to the mass ratio of the tartary buckwheat powder to the extracting solution of 1: 10, placing the tartary buckwheat powder into the extracting solution with the pH value of 8.8, extracting for 0.5h at room temperature, and filtering to obtain the tartary buckwheat extracting solution, wherein the extracting solution comprises the following components: ethanol, sodium sulfite and water; the volume concentration of ethanol in the extracting solution is 60 percent, and the mass concentration of sodium sulfite is 0.2 percent;
(c) adjusting the pH value of the tartary buckwheat extracting solution to 3.5, standing for 5 hours, and filtering to obtain a tartary buckwheat rutin crude product;
(d) and (3) washing the buckwheat rutin crude product with water, and drying in vacuum to obtain the buckwheat rutin.
Example 2
The embodiment is a method for extracting buckwheat rutin, which comprises the following steps:
(a) selecting fresh tartary buckwheat leaves in the flowering period, and then carrying out freeze grinding on the tartary buckwheat leaves for 0.4h to obtain tartary buckwheat powder;
(b) under the ultrasonic condition of 700W, according to the mass ratio of the tartary buckwheat powder to the extracting solution of 1: 10, placing the tartary buckwheat powder into the extracting solution with the pH value of 9.1, extracting for 0.8h at room temperature, and filtering to obtain the tartary buckwheat extracting solution, wherein the extracting solution comprises the following components: ethanol, sodium sulfite and water; the volume concentration of ethanol in the extracting solution is 60 percent, and the mass concentration of sodium sulfite is 0.3 percent;
(c) adjusting the pH value of the tartary buckwheat extracting solution to 2.7, standing for 6 hours, and filtering to obtain a tartary buckwheat rutin crude product;
(d) and (3) washing the buckwheat rutin crude product with water, and drying in vacuum to obtain the buckwheat rutin.
Example 3
The embodiment is a method for extracting buckwheat rutin, which comprises the following steps:
(a) selecting fresh tartary buckwheat stems in a flowering period, and then freezing and grinding the tartary buckwheat stems for 0.5h to obtain tartary buckwheat powder;
(b) under the ultrasonic condition of 800W, according to the mass ratio of the tartary buckwheat powder to the extracting solution of 1: 10, placing the tartary buckwheat powder into the extracting solution with the pH value of 9.3, extracting for 1 hour at room temperature, and filtering to obtain the tartary buckwheat extracting solution, wherein the extracting solution comprises the following components: ethanol, sodium sulfite and water; the volume concentration of ethanol in the extracting solution is 60 percent, and the mass concentration of sodium sulfite is 0.25 percent;
(c) adjusting the pH value of the tartary buckwheat extracting solution to 3.0, standing for 6 hours, and filtering to obtain a tartary buckwheat rutin crude product;
(d) and (3) washing the buckwheat rutin crude product with water, and drying in vacuum to obtain the buckwheat rutin.
Example 4
The embodiment is a method for extracting buckwheat rutin, which comprises the following steps:
(a) selecting fresh tartary buckwheat flowers, leaves and stems in a flowering period, wherein the mass ratio of the flowers, the leaves and the stems is 1: 2: 4; then carrying out freeze grinding on the tartary buckwheat flowers, leaves and stems for 0.5h to obtain tartary buckwheat powder;
(b) under the ultrasonic condition of 800W, according to the mass ratio of the tartary buckwheat powder to the extracting solution of 1: 10, placing the tartary buckwheat powder into the extracting solution with the pH value of 9.0, extracting for 1 hour at room temperature, and filtering to obtain the tartary buckwheat extracting solution, wherein the extracting solution comprises the following components: ethanol, sodium sulfite and water; the volume concentration of ethanol in the extracting solution is 60 percent, and the mass concentration of sodium sulfite is 0.3 percent;
(c) adjusting the pH value of the tartary buckwheat extracting solution to 2.6, standing for 6 hours, and filtering to obtain a tartary buckwheat rutin crude product;
(d) and (3) washing the buckwheat rutin crude product with water, and drying in vacuum to obtain the buckwheat rutin.
Comparative example 1
The comparison example is an extraction method of buckwheat rutin, which is basically the same as the extraction method of the example 1, and the difference is that the buckwheat flower is not subjected to freezing and grinding treatment in the step (a).
Comparative example 2
The comparison example is an extraction method of tartary buckwheat rutin, which is basically the same as the extraction method in the example 1, and the difference is that sodium sulfite is not included in the extracting solution in the step (b).
Examples of the experiments
Extracting the buckwheat rutin in the buckwheat seeds by adopting the extraction methods in the embodiments 1-4 and the comparison examples 1-2 respectively, and then calculating the yield according to the buckwheat rutin/buckwheat tissue multiplied by 100 percent; the calculation results are shown in table 1:
the purity of the tartary buckwheat rutin extracted by different methods is measured by adopting a spectrophotometry method, and the measurement result is shown in the table 1:
TABLE 1 yield and purity of Tartary buckwheat rutin
| Group of | Yield (%) | Purity (%) |
| Example 1 | 6.52 | 98.9 |
| Example 2 | 5.49 | 97.8 |
| Example 3 | 1.68 | 98.3 |
| Example 4 | 3.57 | 98.2 |
| Control ofExample 1 | 5.61 | 98.6 |
| Comparative example 2 | 5.86 | 98.5 |
From the data in table 1:
the extraction method provided by the embodiment of the application can be used for better extracting the tartary buckwheat rutin in the tartary buckwheat tissue, and the extraction rate of the tartary buckwheat rutin is remarkably improved.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (8)
1. The method for extracting the buckwheat rutin is characterized by comprising the following steps:
(a) freezing and grinding the tartary buckwheat tissues to obtain tartary buckwheat powder;
(b) under the ultrasonic condition, the tartary buckwheat powder is placed in an extracting solution with the pH value of 8.5-9.5 for extraction and filtration to obtain a tartary buckwheat extracting solution, wherein the extracting solution comprises the following components: ethanol, sodium sulfite and water;
(c) adjusting the pH value of the tartary buckwheat extracting solution to 2.5-3.5, standing and filtering to obtain a tartary buckwheat rutin crude product;
(d) and (3) washing the buckwheat rutin crude product with water, and drying in vacuum to obtain the buckwheat rutin.
2. The extraction method according to claim 1, wherein in the step (b), the volume concentration of ethanol in the extracting solution is 50-70%, and the mass concentration of sodium sulfite is 0.2-0.3%.
3. The extraction method according to claim 1, wherein in the step (b), the mass ratio of the tartary buckwheat powder to the extracting solution is 1: 8-12.
4. The extraction method according to claim 1, wherein in the step (b), the extraction temperature is room temperature, and the extraction time is 0.5-1 h.
5. The extraction method according to claim 1, wherein in the step (b), the ultrasonic power is 600-800W.
6. The extraction method according to claim 1, wherein in the step (a), the grinding time is 0.2-0.5 h.
7. The extraction method according to claim 1, wherein in the step (a), the tartary buckwheat tissue is at least one of fresh tartary buckwheat flowers, leaves and stems in the flowering period.
8. The extraction method according to claim 1, wherein the standing time in the step (c) is not less than 2 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210705847.4A CN115109108A (en) | 2022-06-21 | 2022-06-21 | Method for extracting buckwheat rutin |
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Citations (9)
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|---|---|---|---|---|
| CN102718820A (en) * | 2012-07-10 | 2012-10-10 | 刘志强 | Method for extracting and refining rutin |
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