CN114404508A - Preparation method of Meyer sedge extract - Google Patents

Preparation method of Meyer sedge extract Download PDF

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CN114404508A
CN114404508A CN202210165437.5A CN202210165437A CN114404508A CN 114404508 A CN114404508 A CN 114404508A CN 202210165437 A CN202210165437 A CN 202210165437A CN 114404508 A CN114404508 A CN 114404508A
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extract
filtrate
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鞠志新
史春凤
范文忠
冯立超
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Jilin Agricultural Science and Technology College
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K36/18Magnoliophyta (angiosperms)
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    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH

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Abstract

The invention relates to the technical field of natural product extraction, in particular to a preparation method of a carex meyeriana extract, which comprises the following steps: s1, cleaning and draining fresh Meyer sedge, and micronizing to 200 meshes to obtain Meyer sedge powder; s2, placing the obtained carex meyeriana powder in a high-pressure reaction kettle, adding a proper amount of deionized water, carrying out ultrasonic enhanced subcritical water extraction treatment for 40-60 min, filtering, keeping filter residues for later use, taking filtrate, and carrying out AB-8 macroporous adsorption resin purification treatment to obtain an extracting solution; s3, placing the obtained filter residue in an ultrahigh pressure homogenizer, adding a proper amount of 48-55% ethanol solution, homogenizing under high pressure, and then carrying out centrifugal separation to obtain supernatant and filter residue; s4, mixing the obtained extract and the filtrate, concentrating in vacuum, and drying to obtain the extract. The method can obviously improve the extraction rate of the carex meyeriana extract (including total flavonoids and polysaccharides), and can avoid the waste of carex meyeriana fibers.

Description

Preparation method of Meyer sedge extract
Technical Field
The invention relates to the technical field of natural product extraction, in particular to a preparation method of a carex meyeriana extract.
Background
Wula sedge (academic name:Carex meyeriana) Also called carex meyeriana, is a multi-fiber plant, contains less three nutrient substances, and the accumulation of dry substances is mainly volatile oil and flavonoid substances. In northeast, the Meyer sedge is usually used as a material for manufacturing straw shoes, bedding, artificial cotton, fiberboards, straw plaited artware, paper and the like, or used for extracting and manufacturing Meyer sedge essential oil, and the Meyer sedge is not fully processed and utilized.
Modern researches find that the wula sedge extract has the effects of clearing and activating the channels and collaterals, eliminating fatigue, improving blood microcirculation, improving immunity, resisting bacteria, resisting inflammation and resisting oxidation, but the existing water extraction process and alcohol extraction process generally have the condition of low extraction rate in the process of preparing the wula sedge extract.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a carex meyeriana extract, which can obviously improve the extraction rate of the carex meyeriana extract (including total flavonoids and polysaccharides).
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a Meyer sedge extract comprises the following steps:
s1, cleaning and draining fresh Meyer sedge, and micronizing to 200 meshes to obtain Meyer sedge powder;
s2, placing the obtained carex meyeriana powder in a high-pressure reaction kettle, adding a proper amount of deionized water, carrying out ultrasonic enhanced subcritical water extraction treatment for 40-60 min, filtering, keeping filter residues for later use, taking filtrate, and carrying out AB-8 macroporous adsorption resin purification treatment to obtain an extracting solution;
s3, placing the obtained filter residue in an ultrahigh pressure homogenizer, adding a proper amount of 48-55% ethanol solution, homogenizing under high pressure, and then carrying out centrifugal separation to obtain supernatant and filter residue;
s4, mixing the obtained extract and the filtrate, concentrating in vacuum, and drying to obtain the extract.
Further, in the step S2, deionized water is added according to a material-liquid ratio of 1: 6-10, the ultrasonic power is 150-200W, the ultrasonic frequency is 50-100 KHz, the pressure is 30-50 MPa, and the extraction temperature is 100-120 ℃.
Further, in the step S3, an ethanol solution is added according to a ratio of material to liquid of 1: 10-20, the pressure of high-pressure homogenization treatment is 50-70 MPa, the treatment flow rate is 5-6L/h, the temperature of the filtrate is 50-70 ℃, and the circulation treatment is carried out for 2-3 times.
Further, still include: and (2) placing the obtained filter residue in an enzymolysis tank, adding 5-6 times of water, adding a-amylase according to the mass percent of 10%, carrying out enzymolysis for 1h at 30-37 ℃, adding pectinase according to the mass percent of 15%, carrying out enzymolysis for 10h at 37-45 ℃, adding protease according to the mass percent of 10%, and carrying out enzymolysis for 1h at 35-37 ℃ to obtain an enzymolysis solution.
Further, still include: mixing the obtained extractive solution, filtrate, and enzymolysis solution, vacuum concentrating, and drying to obtain extract.
The invention has the following beneficial effects:
can remarkably improve the extraction rate of the Meyer sedge extract (comprising total flavone and polysaccharide) and simultaneously can avoid the waste of Meyer sedge fiber.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described in detail below with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A preparation method of a Meyer sedge extract comprises the following steps:
s1, cleaning and draining fresh Meyer sedge, and micronizing to 200 meshes to obtain Meyer sedge powder;
s2, placing the obtained carex meyeriana powder in a high-pressure reaction kettle, adding deionized water according to the material-liquid ratio of 1:8, carrying out ultrasonic strengthening subcritical water extraction treatment for 50 min under the conditions of ultrasonic power of 175W, ultrasonic frequency of 75KHz, pressure of 40MPa and extraction temperature of 110 ℃, filtering, keeping filter residues for later use, taking filtrate, and carrying out AB-8 macroporous adsorption resin purification treatment (the elution volume is 2.74 BV, the flow rate is 1.88 BV/h, and the sample concentration is 2.1 mg/mL) to obtain an extracting solution;
s3, placing the obtained filter residue in an ultrahigh pressure homogenizer, adding 50% ethanol solution according to the ratio of material to liquid of 1:15, carrying out high-pressure homogenization circulation treatment for 2 times under the conditions that the pressure is 60MPa, the treatment flow rate is 5.5L/h, the temperature of the filtrate is between 60 ℃, and carrying out centrifugal separation to obtain supernatant and filter residue;
s4, mixing the obtained extract and the filtrate, vacuum concentrating, and freeze drying to obtain the extract.
Example 2
A preparation method of a Meyer sedge extract comprises the following steps:
s1, cleaning and draining fresh Meyer sedge, and micronizing to 200 meshes to obtain Meyer sedge powder;
s2, placing the obtained carex meyeriana powder in a high-pressure reaction kettle, adding deionized water according to the material-liquid ratio of 1:6, carrying out ultrasonic strengthening subcritical water extraction treatment for 60 min under the conditions of ultrasonic power of 150W, ultrasonic frequency of 50KHz, pressure of 30MPa and extraction temperature of 100 ℃, filtering, keeping filter residues for later use, taking filtrate, and carrying out AB-8 macroporous adsorption resin purification treatment (the elution volume is 2.74 BV, the flow rate is 1.88 BV/h, and the sample concentration is 2.1 mg/mL) to obtain an extracting solution;
s3, placing the obtained filter residue in an ultrahigh pressure homogenizer, adding 48% ethanol solution according to the material-liquid ratio of 1:10, carrying out high-pressure homogenization circulation treatment for 3 times under the conditions that the pressure is 50MPa, the treatment flow rate is 5L/h, the temperature of the filtrate is 50 ℃, and carrying out centrifugal separation to obtain supernatant and filter residue;
s4, mixing the obtained extract and the filtrate, vacuum concentrating, and freeze drying to constant weight to obtain the extract.
Example 3
S1, cleaning and draining fresh Meyer sedge, and micronizing to 200 meshes to obtain Meyer sedge powder;
s2, placing the obtained carex meyeriana powder in a high-pressure reaction kettle, adding deionized water according to the material-liquid ratio of 10, carrying out ultrasonic strengthening subcritical water extraction treatment for 40min under the conditions of ultrasonic power of 200W, ultrasonic frequency of 100KHz, pressure of 50MPa and extraction temperature of 120 ℃, filtering, reserving filter residues, taking filtrate, and carrying out AB-8 macroporous adsorption resin purification treatment (the elution volume is 2.74 BV, the flow rate is 1.88 BV/h, and the sample concentration is 2.1 mg/mL) to obtain an extracting solution;
s3, placing the obtained filter residue in an ultrahigh pressure homogenizer, adding 55% ethanol solution according to the ratio of 20, wherein the pressure is 70MPa, the processing flow rate is 6L/h, the temperature of the filtrate is 70 ℃, performing high-pressure homogenization and circulation processing for 2 times, and performing centrifugal separation to obtain supernatant and filter residue;
s4, mixing the obtained extract and the filtrate, concentrating in vacuum, and drying to obtain the extract.
Example 4
A preparation method of a Meyer sedge extract comprises the following steps:
s1, cleaning and draining fresh Meyer sedge, and micronizing to 200 meshes to obtain Meyer sedge powder;
s2, placing the obtained carex meyeriana powder in a high-pressure reaction kettle, adding deionized water according to the material-liquid ratio of 1:8, carrying out ultrasonic enhanced subcritical water extraction treatment for 50 min under the conditions of ultrasonic power of 175W, ultrasonic frequency of 175KHz, pressure of 40MPa and extraction temperature of 110 ℃, filtering, keeping filter residues for later use, taking filtrate, and purifying with AB-8 macroporous adsorption resin to obtain an extracting solution;
s3, placing the obtained filter residue in an ultrahigh pressure homogenizer, adding 50% ethanol solution according to the ratio of material to liquid of 1: 10-20, carrying out high-pressure homogenization circulation treatment for 2 times under the conditions that the pressure is 60MPa, the treatment flow rate is 5.5L/h, the temperature of the filtrate is 60 ℃, and carrying out centrifugal separation to obtain supernatant and filter residue;
s4, placing the obtained filter residue in an enzymolysis tank, adding 5.5 times of water, adding alpha-amylase according to the mass percent of 10%, carrying out enzymolysis for 1h at 37 ℃, adding pectinase according to the mass percent of 15%, carrying out enzymolysis for 10h at 45 ℃, adding protease according to the mass percent of 10%, and carrying out enzymolysis for 1h at 37 ℃ to obtain an enzymolysis solution;
s5, mixing the obtained extract, filtrate and enzymolysis liquid, vacuum concentrating, and drying to obtain the extract.
Comparative example 1
A preparation method of Meyer sedge polysaccharide comprises the following steps:
s1, washing and draining fresh wula sedge which is equal to the amount in the embodiment 1, and then micronizing to 200 meshes to obtain wula sedge powder;
s2, placing the obtained carex meyeriana powder in an extraction tank, adding deionized water according to the material-liquid ratio of 1:8, extracting at 90 ℃, filtering after 1.6 h, taking filter residue for later use, taking filtrate, purifying with AB-8 macroporous adsorption resin (the elution volume is 2.74 BV, the flow rate is 1.88 BV/h, and the sample concentration is 2.1 mg/mL), obtaining an extracting solution, and freeze-drying to constant weight.
Comparative example 2
A preparation method of Meyer sedge total flavonoids comprises the following steps:
s1, washing and draining fresh wula sedge which is equal to the amount in the embodiment 1, and then micronizing to 200 meshes to obtain wula sedge powder;
s2, placing the obtained carex meyeriana powder in an extraction tank, adding 50% ethanol solution according to the material-liquid ratio of 1:30, extracting at 70 ℃ for 90min to obtain an extracting solution, and freeze-drying to constant weight.
The total flavone content and polysaccharide content in example 1 were determined, while the polysaccharide content in comparative example 1 and total flavone content in comparative example 2 were determined, wherein:
determination of total flavone content
Diluting the sample solution by 10 times, transferring the sample solution into a measuring cylinder, and accurately measuring the volume of the sample solution to be used as stock solution for measuring the content of the total flavonoids in the carex meyeriana. Transferring 1mL of the stock solution by a pipette, adding the stock solution into a test tube, and adding 5% NaNO20.30mL of the aqueous solution (3), sufficiently shaken, and left to stand for 6 min, followed by adding 0.30mL of 10% Al (NO) thereto3)3Shaking the aqueous solution to fully react, standing for 6 min, finally adding 4.00 mL of 4% NaOH aqueous solution, adding 80% ethanol solution to constant volume to 10.00 mL, fully shaking, standing for 15min, and taking the volume fraction as the volume fractionAnd (3) carrying out blank reference blank zero adjustment on 80% ethanol solution, and measuring the absorbance of the component to be measured by using an ultraviolet spectrophotometer at the wavelength of 510 nm. Taking rutin as a standard substance, and according to a regression equation of absorbance (Y) and concentration (X): y is 14.548 x-0.0113, R2 is 0.9997, and the content of the total flavonoids is = the mass of the total flavonoids/the mass of the carex meyeriana powder.
Determination of polysaccharide content
Phenol-sulfuric acid colorimetry is adopted. The sample solution was diluted 30-fold, 0.5mL of the diluted solution was transferred to a test tube, and 1mL of a 5% phenol solution and 3.5mL of concentrated H were added2SO4Shaking, mixing, treating the mixture in water bath at 40 deg.C for 30min, cooling at room temperature for 15min, and measuring absorbance at 490 nm. The blank solution was made with distilled water instead of sample diluent and the glucose standard curve was y =6.6671x + 0.0202.
As a result: the extraction rate of the total flavone in the example 1 is obviously higher than that in the comparative example 2, and is respectively 8.17 percent and 6.21 percent; the polysaccharide extraction rate was significantly higher than comparative example 1, 0.81% and 0.45%, respectively.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.

Claims (5)

1. A preparation method of a Meyer sedge extract is characterized in that: the method comprises the following steps:
s1, cleaning and draining fresh Meyer sedge, and micronizing to 200 meshes to obtain Meyer sedge powder;
s2, placing the obtained carex meyeriana powder in a high-pressure reaction kettle, adding a proper amount of deionized water, carrying out ultrasonic enhanced subcritical water extraction treatment for 40-60 min, filtering, keeping filter residues for later use, taking filtrate, and carrying out AB-8 macroporous adsorption resin purification treatment to obtain an extracting solution;
s3, placing the obtained filter residue in an ultrahigh pressure homogenizer, adding a proper amount of 48-55% ethanol solution, homogenizing under high pressure, and then carrying out centrifugal separation to obtain supernatant and filter residue;
s4, mixing the obtained extract and the filtrate, concentrating in vacuum, and drying to obtain the extract.
2. The method of claim 1, wherein the method comprises the steps of: in the step S2, deionized water is added according to the ratio of material to liquid of 1: 6-10, the ultrasonic power is 150-200W, the ultrasonic frequency is 50-100 KHz, the pressure is 30-50 MPa, and the extraction temperature is 100-120 ℃.
3. The method of claim 1, wherein the method comprises the steps of: in the step S3, an ethanol solution is added according to a material-liquid ratio of 1: 10-20, the pressure of high-pressure homogenization treatment is 50-70 MPa, the treatment flow rate is 5-6L/h, the temperature of the filtrate is 50-70 ℃, and the circulation treatment is carried out for 2-3 times.
4. The method of claim 1, wherein the method comprises the steps of: further comprising: and (2) placing the obtained filter residue in an enzymolysis tank, adding 5-6 times of water, adding a-amylase according to the mass percent of 10%, carrying out enzymolysis for 1h at 30-37 ℃, adding pectinase according to the mass percent of 15%, carrying out enzymolysis for 10h at 37-45 ℃, adding protease according to the mass percent of 10%, and carrying out enzymolysis for 1h at 35-37 ℃ to obtain an enzymolysis solution.
5. The method of claim 4, wherein the method comprises the steps of: further comprising: mixing the obtained extractive solution, filtrate, and enzymolysis solution, vacuum concentrating, and drying to obtain extract.
CN202210165437.5A 2022-02-23 2022-02-23 Preparation method of Meyer sedge extract Pending CN114404508A (en)

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Application publication date: 20220429