CN113521795A

CN113521795A - Extraction method and application of purple yam active substances

Info

Publication number: CN113521795A
Application number: CN202010306504.1A
Authority: CN
Inventors: 郑长义
Original assignee: Individual
Current assignee: Individual
Priority date: 2020-04-17
Filing date: 2020-04-17
Publication date: 2021-10-22

Abstract

The invention relates to an extraction method and application of purple yam active substances, which is characterized by applying supercritical CO₂Extraction method (Supererical CO)₂Preprocessing) "to extract active substances contained in the roots and stems of purple yam (Dioscore Rhizoma Thunb), such as active substances like cysteamine Peroxidase cofactor (glutamon Peroxidase enzymes) and longevity protein (Klotho), and to add Glyconutrients (glyconutrints) for the purpose of activating and providing in vivo cell nutrients, therefore, the extraction process of the present invention is simple and time-saving, and uses CO₂The solvent has low critical temperature and pressure, can be recycled, and has low cost, high extraction rate and application value.

Description

Extraction method and application of purple yam active substances

Technical Field

The invention relates to an extraction method and application, in particular to a method for extracting supercritical CO₂Extraction method (Supererical CO)₂Preprocessing) "to extract purple yam (Dioscore Rhizoma thunnb: DRT) active substance contained in the rhizome; and an extraction method and application of purple yam active substances for activating in vivo cells and providing in vivo cell nutrients by matching the extract with 'carbohydrate nutrients'.

Background

According to the invention patent of the Chinese yam low molecular extract and the preparation method thereof which is specially issued on 21.3.2007 in Taiwan (application number: 092136872, certificate number: I276440) and the invention patent of the Chinese yam extract and the pharmaceutical composition thereof which is issued on 21.7.2011 in 2011 (application number: 093135192, certificate number: I345471), the method is to combine the extract with the interleukin 2 to form the pharmaceutical mixture by the traditional processes of adding acid, adding alcohol, removing solvent, filtering, distilling and the like, and the process is complex and time-consuming and has low extraction rate; in addition, the common yam refers to a strain (Dioscorea Opposita Thunb) with white rhizome, which contains saponin, dopamine, dioscin, polyphenol oxidase and other beneficial health components, and is commonly called 'Huaishan' in traditional Chinese medicine, and beneficial to spleen and stomach health; the other yam strain (Dioscorea Rhizoma Thunb) has purple root and stem, is called purple yam, contains special active substances such as cysteamine peroxidase cofactor (GPC), main components Quercetin-3-0-rutinose (Q30) and jopsin (Klotho), and the like, is sensitive to heat, and can be damaged when the temperature is higher than 40 ℃; in addition, carbohydrate nutrients were discovered by the 1999 nobel biomedical winner, bramberber bosch (dr. gunther blob): carbohydrate (a carbohydrate chain formed by combining carbohydrate nutrients with proteins or lipids) has important functions in the transmission and communication of cellular messages, and essential monosaccharides and carbohydrate (sugar codes) contained in carbohydrate nutrients (Glyco-nutrients) constitute nutrients which have healthy and complete cell receptor functions and make various tissues and organs function normally and indispensable, and confirm that cell aging, pathological changes, diseases, cancers and carbohydrate are closely related; symptom of glycobody incompetence: if the carbohydrate is not complete, the cell function is not properly functioning, and the body will develop four conditions: (1) failure to absorb or over-absorb nutrients, which can lead to diabetes, cancer, osteoporosis, anemia and other diseases; (2) the intercellular wastes can not be successfully removed, which can cause diseases such as hypertension, gout and the like; (3) failure to identify autologous cells or foreign bacteria and viruses will lead to hypoimmunity, allergy, asthma, lupus erythematosus and rheumatoid arthritis; (4) failure of cells and tissues to coordinate with each other can lead to insomnia, infertility, endocrine disorders, and depression. At present, the existing method uses the traditional processes of adding acid, adding alcohol, removing solvent, filtering, distilling and the like to obtain the yam extract, and then combines the yam extract with the interleukin 2 to form a medicinal mixture, and the process is complex and time-consuming and has low acquisition rate, so that the popularization is not seen, the practicability of the yam extract is greatly reduced, and the problem that the technicians and consumers in the field want to solve is solved.

Disclosure of Invention

In order to solve the defects of the prior art, the invention mainly aims to provide an extraction method and application of purple yam active substances, and supercritical CO is adopted₂Extraction method (Supererical CO)₂Preprocessing) to extract active substances contained in the purple yam rhizome, in order to overcome the problems in the prior art.

The invention also aims to provide an extraction method and application of the purple yam active substances, which can achieve the purposes of activating in-vivo cells and supplementing in-vivo cell nutrients by utilizing active substance extracts contained in the extracted purple yam rhizome and matching with carbohydrate nutrients (glyconutants) to be applied to the results of a white mouse diet test.

The invention aims to provide an extraction method and application of purple yam active substances, the extraction process is simple and time-saving, the solvent critical temperature and pressure are low, the solvent can be recycled, the cost is low, and the extraction rate is high and safe.

The problem to be solved by the invention is that according to the taiwan patent application number in the prior art: no. 092136872, certificate number: the invention patent and application number of 'Chinese yam low molecular extract and preparation method' of I276440: 093135192, certificate number: the invention of the invention patent of 'Chinese yam extract and its pharmaceutical composition' of I345471 is a method of combining the extract obtained by the conventional processes of adding acid, adding alcohol, removing solvent, filtering, distilling and the like with interleukin 2 to form a pharmaceutical mixture, which is complicated and time-consuming and has low extraction rate, thus having no practicability.

The technical means for solving the problems is to achieve the aim, the invention provides an extraction method and application of purple yam active substances, and the method is characterized in that supercritical CO is adopted₂Extraction method (Supererical CO)₂Preworking) "includes the steps in the order:

peeling the Chinese yam, cutting into blocks, placing the blocks into a raw material barrel, and standing for ten minutes to stabilize active substances contained in the Chinese yam.

And (II) putting the Chinese yam peeled and cut in the step (I) into an extraction pot, connecting the extraction pot with a solvent circulating pump for providing a solvent, putting the Chinese yam into the extraction pot for first extraction, and putting the Chinese yam into an extraction barrel.

And (III) after the Chinese yams peeled and cut in the step (II) are put into an extraction pot for first extraction, the Chinese yams are put into an extraction barrel for thirty minutes and then are depressurized, and after extraction is stopped, the Chinese yams are put into a first separation pot for separation into carbohydrates with the upper layer being active substances with light specific gravity and the lower layer being heavy specific gravity.

And (IV) putting the active substances with light specific gravity at the upper layer of the carbohydrates separated and removed by the first separation pot in the second separation pot.

And (V) depressurizing the active substances on the upper layer separated by the first separation pot in the step (IV) after a period of time, stopping extraction, and separating in the second separation pot.

And (VI) decomposing the active substance components with the specific gravity of less than 1.0 in the second separation pot in the step (five), filtering the circulating solvent through a low-pressure filter, and providing the condensed solvent to enter the solvent storage barrel so as to recycle and reuse in the separation process.

Further, the yam in the step (one) of the present invention is purple yam (Dioscorea rhizozoma Thunb).

Further, a solvent preheater is arranged between the extraction pot and the solvent circulating pump in the step (II).

Further, the active substance ingredient of the step (III) of the present invention is light specific gravity bran cystamine Peroxidase cofactor (glutathione Peroxidase: GPC), the main ingredients of which are Quercetin-3-0-rutinose (Q30) and longevity protein (Klotho).

Further, a high-pressure filter and a first separation preheater are sequentially and serially arranged between the extraction barrel and the first separation pot in the step (III).

Furthermore, a circulating solvent dryer is arranged between the circulating solvent cooler in the step (six) and the circulating solvent cooler, the solvent storage barrel is connected with a vacuum pump, and the circulating solvent dryer is used for removing water in the circulating solvent so as to reduce the influence on the extraction rate caused by the generation of the non-condensable solvent in the system.

Further, a second preheating separator is arranged between the first separating pot and the second separating pot in the step (IV).

Further, the first separation pot and the second separation pot in the step (four) of the present invention are respectively connected to a first product tank (low pressure), a first product pump and a second product pump and are simultaneously connected to a finished product storage tank.

Further, the solvent of the step (two) of the present invention is CO₂。

The technical means for solving the problems is to achieve the purpose, and the invention provides the extraction application of the purple yam active substance, which is characterized in that the active substance extracted from the yam is matched with carbohydrate nutrients (glyconutants) to provide the purposes of activating the cells in the white mouse and providing the nutrients for the cells in the white mouse.

Further, the yam of the present invention is purple yam (Dioscorea Rhizoma Thunb).

Furthermore, the active substances extracted from the purple yam of the invention are matched with carbohydrate nutrients (glyconutants), and are used for the white mouse diet test.

Compared with the prior art, the invention adopts supercritical CO₂Extraction method (Supererical CO)₂Preprocessing) to extract active substances contained in the purple yam rhizome, and matching with carbohydrate nutrients (glyconutants) to perform a white mouse diet test, so that the purposes of activating in vivo cells and supplementing in vivo cell nutrients can be achieved; effectively improves the extraction process, ensures that the extraction process is simple and time-saving, has low solvent critical temperature and pressure, can be recycled, has low cost and high extraction rate, is safe, can greatly expand the industrial utilization and has novelty and creativity.

Drawings

FIG. 1 is a flow chart of the extraction process of the present invention.

FIG. 2 is a drawing of the peeled purple yam of the present invention.

FIG. 3 is a diagram of a peeled purple yam of the present invention.

Detailed Description

The present invention will now be described in detail with reference to the drawings and embodiments, and the drawings used herein are for illustrative purposes only and are not necessarily to scale or precise configuration after the practice of the invention, and therefore the scope of the invention should not be limited by the scale and configuration of the drawings.

FIG. 1 is a flow chart of the extraction method of the present invention, FIG. 2 is a drawing of peeled purple yam of the present invention, FIG. 3 is a drawing of peeled purple yam of the present invention, and the extraction method of active substances of purple yam of the present invention and its application in a preferred embodiment are characterized by using supercritical CO₂Extraction method (Supererical CO)₂Preprocessing) ", comprising the steps in the order:

peeling purple Chinese yam, cutting into pieces, placing the pieces into a raw material barrel, and standing for 10-30 minutes to stabilize active substances contained in the Chinese yam (as shown in figure 1); the peeled yam obtained in the first step of this example is purple yam (Dioscorea rhizome Thunb) M (the shape is shown in FIG. 2, and the shape is shown in FIG. 3), but the present invention is not limited thereto, and the peeled yam is cut into 5cm pieces, and the peeled yam pieces are put into a raw material barrel for a standing time of at least ten minutes, in this example thirty minutes, but the present invention is not limited thereto.

Secondly, placing the purple yam peeled and cut in the step one into an extraction pot A-1, connecting the extraction pot A-1 with a solvent circulating pump Q-1 for solvent passing, placing the purple yam into the extraction pot A-1 for primary extraction, and then placing the purple yam into an extraction barrel A-2; in this embodiment, the extraction pot A-1 has a capacity of 1m³An extraction apparatus, but not limiting the invention thereto, is provided with a solvent preheater Q-2 between the extraction pot A-1 and the solvent circulation pump Q-1, the temperature of the extraction pot A-1 is 31 deg.C, the pressure is 7.39MPa, the solvent is CO in this embodiment₂Solvent (as shown in figure 1)Shown).

(III) putting the purple Chinese yams which are peeled and cut into blocks in the step (II) into an extraction pot A-1 for first extraction, putting the purple Chinese yams into an extraction barrel A-2 for a period of time, and then reducing the pressure, wherein the pressure is reduced after the period of time is at least thirty minutes, and the pressure is reduced after 1 hour in the embodiment, but the invention is not limited by the step, and after extraction is stopped, putting the purple Chinese yams into a first separation pot C-1 for separation into carbohydrates with the upper layer being light active substances and the lower layer being heavier; in this embodiment, the active substance component is light specific gravity Glutathione Peroxidase Cofactors (GPC), the main components of the said glutathione Peroxidase cofactors are Quercetin-3-0-rutinose (Q30) and joistin (Klotho), the pressure of the first separation pot C-1 is 6.5MPa, but the invention is not limited by this, and in addition, a high pressure filter F-1 and a first separation preheater B-1 (as shown in FIG. 1) are connected in series between the extraction barrel A-2 and the first separation pot C-1.

(IV) placing the lighter active substance containing upper layer of carbohydrate separated and removed by the first separation pot C-1 in the step (III) into a second separation pot C-2; in this embodiment, the temperature of the second separation pot C-2 is 31 ℃, the pressure is 7.39Mpa, a second preheating separator B-2 is arranged between the first separation pot C-1 and the second separation pot C-2, the first separation pot C-1 and the second separation pot C-2 are respectively connected with a first product barrel (low pressure) D-1, a first product pump P-1, a second product barrel D-2, and a second product pump P-2, and the first product pump P-1 and the second product pump P-2 are simultaneously connected with a finished product storage barrel (as shown in FIG. 1).

Fifthly, reducing the pressure of the active substances in the upper layer separated by the first separation pot C-1 in the step (four) after a period of time, wherein the pressure is reduced for at least thirty minutes after the period of time, and the pressure is reduced after the period of time is 1 hour in the embodiment, but the invention is not limited by the step, and the separation is carried out in the second separation pot C-2 after the extraction is stopped; in this embodiment, the second separation pot C-2 is depressurized after one hour and then the extraction is stopped, and the pressure of the second separation pot C-2 is 6.0MPa (as shown in FIG. 1).

(VI) the step (five)) The second separation pot C-2 decomposes active material components with a specific gravity of 1.0 or less, and in the separation process, the circulating solvent is filtered by a low-pressure filter F-2 and a circulating solvent cooler E-1 and a circulating solvent cooler E-2 are provided to condense the solvent and enter the solvent storage barrel S-1 for recycling; a circulating solvent drier K-1 is arranged between the circulating solvent cooler E-1 and the circulating solvent cooler E-2, the solvent storage barrel S-1 is connected with a vacuum pump VP-1, and the circulating solvent drier K-1 is used for removing moisture in the circulating solvent so as to reduce the influence on the extraction rate caused by the generation of the non-condensable solvent in the system. The separation process of the invention is carried out at near normal temperature (31 ℃) and the CO of the solvent₂The critical temperature of the solvent is 31-32 ℃, and the active substances sensitive to heat are not damaged (as shown in figure 1).

The present invention provides a method for extracting active substances from purple yam and the use thereof, wherein the method is characterized in that the active substances extracted from purple yam are added with carbohydrate nutrients (glyconutrints) to provide in vivo cell nutrients and cell activation, and can slow down the deterioration of age to the cognitive ability of the brain.

Application test

1. Test one: and (3) comparing the blood characteristics of the white mice.

(1) The method comprises the following steps: 30 mice born 90 days old are divided into three groups of 10 mice, and blood is collected after four weeks to analyze the blood characteristics.

A. Control group: compound feed

B. One set of experiments was: matched diet and active substance

C. Two groups of experiments were performed: matched with feed, active substance and carbohydrate nutrient

The food is matched in the way: 40% of wheat germ, 33.3% of millet, 5.0% of fish meal, 7.5% of soybean meal, 5.0% of alfalfa, 2.0% of corn oil, 2.0% of yeast, 1.3% of calcium carbonate and 3.9% of trace elements.

(2) As a result: it is shown in Table 1 that the numbers of both the B, C leukocytes and lymphocytes increased.

The results show that: the extract of the invention and carbohydrate nutrients can improve the immunity of mice.

TABLE 1 analysis of the hematological examination of the mice administered with "active substance

2. And (2) test II: test for Effect on subcutaneous fibroblast content

(1) The method comprises the following steps: 24 mice of 120 days old are divided into three groups of 8 mice.

A. Control group: compound feed (ingredient same test)

B. One set of experiments was: compound feed and active substance (500mg)

C. Two groups of experiments were performed: matching with feed, active substance (500mg), carbohydrate nutrient (500mg)

(2) As a result:

TABLE 2 Effect of active substance administration to mice on their fibroblast content in vivo

A: the fibroblast is larger than the general cell in shape, is in a star shape or a fusiform shape, has a protrusion, has an oval shape of cell nucleus, is sparse in chromosome, is slightly stained, has obviously larger nucleolus and has more cytoplasm. Fibroblasts are capable of synthesizing or secreting collagen to maintain the elasticity of the top skin.

B: collagen, elastin and proteoglycan can form collagen fiber, elastic fiber and reticular fiber, which can increase the toughness of cell membrane of organ and prevent cell damage.

C: fibroblasts are active in function and have the function of accelerating wound healing during the repair of tissue damage.

3. And (3) test III: comparative test for cognitive ability (degeneration) of white mouse brain

(1) Method of producing a composite material

A: control group: the mouse is 10 mice (equivalent to 20 years old) in five months after birth

Control two groups: mouse 10 mice aged eighteen months after birth (equivalent to 65 years old)

Test groups: mouse 10 mice aged eighteen months after birth (equivalent to 65 years old)

B: feed

Control group: the same experiment I and the same basic compound feed

Control two groups: the same experiment I and the same basic compound feed

Test groups: basal compound diet, active substance (500mg), carbohydrate nutrient (500mg)

C: go 5 meters long maze game and calculate the time needed for reaching the terminal station

(2) Results

From the test results, it is found that the feed of 18-month-old white mice (65 years old equivalent to human) contains the purple yam extract active substance and carbohydrate nutrients, and has the effect of delaying the brain cognitive ability deterioration (up to 70%).

The extraction method and application of the purple yam active substance utilize supercritical CO₂Characteristic of the extraction, CO₂In order to replace water or organic solvent as an extraction medium without toxicity and residue and perform extraction at the condition close to room temperature, the advantages are listed as follows:

(1)CO₂colorless, tasteless, nontoxic and generally gas in condition, no solvent residue, absolutely safe and easy to obtain extract by using it as extraction solvent.

(2) The extraction temperature is close to room temperature, and the extraction rate of substances sensitive to humidity, heat, light and the like in the whole extraction separation process is high.

(3) The method has the advantages of simple flow, few steps, short time consumption, high efficiency and capability of omitting certain separation steps of the traditional extraction method.

(4) Supercritical CO₂Has strong dissolving capacity and permeability, high diffusion speed, continuous dynamic condition and complete extraction.

(5)CO₂Only acts on the solute and does not change any components or properties except the solute.

(6)CO₂Low cost, easy obtaining, low critical temperature and critical pressure, easy achievement and recycling in operation and low production cost. The residue after extraction (carbohydrate residue) can also be used as animal feed.

Therefore, the present invention employs supercritical CO₂Extraction method (Supererical CO)₂Preprocessing) to extract active substances contained in the purple yam rhizome; therefore, the functions of activating in-vivo cells and supplementing in-vivo cell nutrients can be achieved by extracting active substance extracts contained in the purple yam rhizome and matching with carbohydrate nutrients (glyconutants) to be applied to a white mouse diet test; effectively improves the extraction process, ensures that the extraction process is simple and time-saving, has low solvent critical temperature and pressure, can be recycled, has low cost and high extraction rate, is safe, can greatly expand the industrial utilization and has novelty and creativity.

The above-described embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and to implement the present invention, and not to limit the scope of the present invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.

Description of the symbols

A-1 … extraction pot;

a-2 … extraction barrel;

b-1 … first separation preheater;

a C-1 … first separation pot;

d-1 … first product bucket (Low pressure);

product pump No. P-1 …;

b-2 … second preheating separator;

a C-2 … second separation pot;

d-2 … second product bucket;

a product pump No. P-2 …;

f-1 … high pressure filter;

f-2 … low-pressure filter;

e-1 … recirculating solvent chiller;

k-1 … circulating solvent drier;

e-2 … recirculating solvent chiller;

s-1 … solvent storage barrel;

VP-1 … vacuum pump;

q-1 … solvent circulation pump;

a solvent preheater of Q-2 …;

m … peeled purple yam.

Claims

1. The extraction method of purple yam active substances is characterized by adopting supercritical CO₂The extraction method comprises the following steps in sequence:

peeling the Chinese yam, cutting into blocks, placing the blocks into a raw material barrel, and standing for at least ten minutes to stabilize active substances contained in the Chinese yam;

placing the Chinese yam peeled and cut into blocks in the step (I) into an extraction pot, wherein the extraction pot is connected with a solvent circulating pump for providing a solvent, and placing the Chinese yam into an extraction pot for first extraction and then into an extraction barrel;

thirdly, after the Chinese yams peeled and cut in the second step are put into an extraction pot for first extraction, the Chinese yams are put into an extraction barrel for thirty minutes and then are depressurized, and after extraction is stopped, the Chinese yams are put into a first separation pot for separation into carbohydrates with the upper layers being active substances with light specific gravity and the lower layers being heavy specific gravity;

putting the active substances with light specific gravity at the upper layer of the carbohydrate separated and removed by the first separation pot in the step (three) into a second separation pot;

fifthly, reducing the pressure of the active substances on the upper layer separated by the first separation pot in the step (four) after thirty minutes, stopping extraction, and separating in the second separation pot;

2. The method for extracting active ingredients of purple yam according to claim 1, wherein the yam of step (a) is purple yam.

3. The method for extracting active ingredients from purple yam according to claim 1, wherein a solvent preheater is arranged between the extraction pot and the solvent circulating pump in the second step.

4. The method for extracting active ingredients from purple yam according to claim 1, wherein the active ingredients in step (three) are light-specific weight glutathione peroxidase cofactor, and the main ingredients of the glutathione peroxidase cofactor are Quercetin-3-0-rutinose and longevity protein.

5. The method for extracting active ingredients from purple yam according to claim 1, wherein a high pressure filter and a first separation preheater are sequentially connected in series between the extraction barrel and the first separation pot in the step (III).

6. The method for extracting active ingredients from purple yam according to claim 1, wherein a circulating solvent dryer is disposed between the circulating solvent cooler and the circulating solvent condenser in the step (six), the solvent storage tank is connected to a vacuum pump, and the circulating solvent dryer provides water to the circulating solvent to reduce the generation of non-condensable solvent in the system and thus to reduce the influence on the extraction rate.

7. The method for extracting active ingredients of purple yam according to claim 1, wherein a second preheating separator is arranged between the first separating pot and the second separating pot in the step (four).

8. The method for extracting active ingredients from purple yam according to claim 1, wherein the first separation pot and the second separation pot of step (IV) are respectively connected with a first product barrel (low pressure), a first product pump, a second product barrel and a second product pump, and the first product pump and the second product pump are simultaneously connected with a finished product storage barrel.

9. The method for extracting active ingredients from purple yam according to any one of claims 1 to 8, wherein the solvent in the second step (II) is CO₂A solvent.

10. An extraction application of purple yam active substances, which is extracted according to the extraction method of purple yam active substances of claims 1 to 8, is used for matching with the addition of carbohydrate nutrients, can provide the functions of activating in-vivo cells and providing in-vivo cell nutrients, can increase the number of white blood cells and lymphocytes in blood, is helpful for improving immunity, increases the number of fibroblasts in the inner layer of skin, is helpful for the synthesis of collagen, is helpful for skin maintenance and delays the phenomenon of age deterioration of the cognitive ability of the brain.