CN114989887A - Complex enzyme assisted supercritical CO 2 Method for extracting houttuynin - Google Patents

Complex enzyme assisted supercritical CO 2 Method for extracting houttuynin Download PDF

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CN114989887A
CN114989887A CN202210537110.6A CN202210537110A CN114989887A CN 114989887 A CN114989887 A CN 114989887A CN 202210537110 A CN202210537110 A CN 202210537110A CN 114989887 A CN114989887 A CN 114989887A
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houttuynia cordata
extracting
extraction
supercritical
enzymolysis
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曾立民
刘小琳
范金凤
徐晓云
吴婷
李有志
刘婷婷
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Hubei Onlylong Food Co ltd
Huazhong Agricultural University
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Hubei Onlylong Food Co ltd
Huazhong Agricultural University
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78—Separation; Purification; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78—Separation; Purification; Stabilisation; Use of additives
    • C07C45/80—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/025—Recovery by solvent extraction
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

The invention belongs to the technical field of extraction of active ingredients of natural products, and particularly relates to compound enzyme-assisted supercritical CO 2 A method for extracting houttuynin comprises cleaning fresh herba Houttuyniae, air drying surface water, cutting, adding complex enzyme for enzymolysis, freeze drying, pulverizing, and performing supercritical CO extraction 2 The houttuynia cordata extract is obtained by extraction and separation, and the process can improve the yield of the houttuynia cordata volatile oil and the content of the houttuynine sodium bisulfite, and has wide application prospect.

Description

Complex enzyme-assisted supercritical CO 2 Method for extracting houttuynin
Technical Field
The invention belongs to the technical field of extraction of active ingredients of natural products, and particularly relates to compound enzyme-assisted supercritical CO 2 A method for extracting houttuynin.
Background
The herba Houttuyniae is houttuynia cordata Thunb of Saururaceae, and has pungent taste, cold and cool nature, and enters lung meridian. It is recorded in the Chinese pharmacopoeia 2015 edition, which has the effects of clearing heat and removing toxicity, resolving carbuncle and discharging pus, inducing diuresis and treating stranguria, and the like, is clinically used for treating lung carbuncle and purulent, phlegm heat and asthma, heat dysentery, heat stranguria, carbuncle swelling and sore toxicity, and the like, is an important medicine for treating lung carbuncle, and is praised as a broad-spectrum antibiotic in traditional Chinese medicines. Research shows that the houttuynia cordata has remarkable activities of resisting inflammation, inhibiting bacteria, resisting viruses, resisting tumors, protecting the liver and the like, is closely related to volatile oil and flavone in the houttuynia cordata, and has remarkable anti-inflammatory effect on decanoyl acetaldehyde (houttuynin) in the volatile oil. However, houttuynin is easily oxidized and decomposed, and is converted into methyl n-nonanone through oxidation and decarboxylation, so that the anti-inflammatory capability of the houttuynin is relatively weak. The prepared volatile oil rich in houttuynine sodium bisulfite can be used for developing products with anti-inflammatory effect, and has wide market prospect. The prior extraction methods of the houttuynia cordata are various, such as a steam distillation method, a solvent extraction method, an enzyme method auxiliary method and the like. The steam distillation method has the advantages that due to high temperature, active ingredients are easy to oxidize and degrade, so that the extraction rate is low and the activity is poor; the solvent extraction method has the advantages of high cost, low product purity, complex working procedures, easy loss of volatile oil and solvent residue. The above extraction methods have low content of houttuynine sodium bisulfite. As a novel extraction technology, the supercritical fluid extraction has the advantages of high mass transfer rate, no solvent residue and simple and convenient product separation, and is widely applied to extraction of natural active substances. Carbon dioxide is favored by many enterprises because of its advantages of safety, environmental protection, non-toxicity, economy, etc.
Disclosure of Invention
The invention mainly solves the defects of low extraction efficiency, damaged active ingredients and complicated process in the existing traditional extraction method, and provides a method for assisting supercritical fluid by using complex enzymeCO 2 Novel combined extraction mode of extraction. The supercritical extraction technology and the enzymolysis reaction are combined to extract and separate active substances such as houttuynin and the like. Aims to provide a method for extracting volatile oil rich in houttuynin, which can prevent the volatile oil from oxidative degradation, has no solvent residue, and has high extraction rate and good purity.
The invention provides the following technical scheme: complex enzyme-assisted supercritical CO 2 The invention relates to a method for extracting houttuynine sodium bisulfite, which comprises the following steps:
step 1: removing impurities from fresh herba Houttuyniae, cleaning fresh herba Houttuyniae, air drying, cutting into segments;
and 2, step: adding compound enzyme into the cut fresh houttuynia cordata for enzymolysis;
and step 3: drying the houttuynia cordata after enzymolysis in a freeze dryer;
and 4, step 4: pulverizing the freeze-dried herba Houttuyniae in a pulverizer;
and 5: pulverizing herba Houttuyniae powder in supercritical CO 2 Extracting in an extraction kettle, and separating in a separation kettle to obtain volatile oil rich in houttuynin;
preferably, the following components: and (2) cleaning the fresh houttuynia cordata by using drinking water in the step 1, placing the cleaned fresh houttuynia cordata in a cool environment until the surface of the fresh houttuynia cordata is dried, and cutting the fresh houttuynia cordata into sections with the lengths of 1-5 mm.
Preferably: in the step 2, the addition amount of the complex enzyme is 1-3% of the mass of the fresh houttuynia cordata.
Preferably: the complex enzyme in the step 2 consists of cellulase and pectinase according to the mass ratio of 1: 1.
Preferably, the following components: in the step 2, the enzymolysis temperature is 40-50 ℃, the enzymolysis pH is 4.5-6.5, and the enzymolysis time is 1-3 h.
Preferably: and in the step 2, the pH value of enzymolysis is adjusted by using 10mg/ml citric acid.
Preferably: and (3) drying the houttuynia cordata in the step 3 in a freeze dryer at the temperature of-20 to-40 ℃ for 12 to 24 hours.
Preferably: and (5) sieving the crushed cordate houttuynia in the step (4) by using a 40-mesh sieve.
Preferably:supercritical CO in said step 5 2 When the houttuynia cordata is extracted, the extraction temperature is 40-50 ℃, the extraction pressure is 15-30 Mpa, the extraction time is 1-3 h, and CO is added 2 The flow rate is 20-30L/h.
Preferably, the following components: the addition amount of the freeze-dried houttuynia cordata powder added into the extraction kettle in the step 5 is 100-200 g, the pressure of the separation kettle is 5-7 MPa, and the temperature of the separation kettle is 40-50 ℃.
Compared with the prior art, the invention has the beneficial effects that:
(1) the mode of combining the supercritical extraction technology and the enzymolysis reaction is adopted, so that the extraction of effective components is accelerated and improved;
(2) freeze vacuum drying the fresh houttuynia cordata, and maximally preserving the medicinal effective components in the fresh houttuynia cordata while drying;
(3) the volatile oil rich in active ingredients such as houttuynin and the like can be obtained by the process, so that a large amount of volatile oil is preserved, the active ingredients such as houttuynin and the like are also rich, and the medicinal effect of the product is enhanced;
(4) the product obtained by supercritical carbon dioxide extraction has no solvent residue and high product purity, and the heat-sensitive and easily-oxidized active ingredients such as houttuynine sodium bisulfite and the like are protected to a great extent.
Detailed Description
The technical solution of the present invention is further specifically described by the following examples, which are illustrative and not restrictive, and the scope of the present invention is not limited by the following examples.
The houttuynine sodium bisulfite is detected by a gas chromatograph, and the content of the houttuynine sodium bisulfite is calculated by a standard yeast method of houttuynine sodium bisulfite.
Example 1
Complex enzyme-assisted supercritical CO 2 The method for extracting the houttuynine sodium bisulfite comprises the following steps:
(1) cleaning fresh houttuynia cordata with drinking water, airing the fresh houttuynia cordata in a cool environment to the surface, and cutting into sections with the length of 1-5 mm;
(2) adding a compound enzyme into the cut fresh houttuynia cordata for enzymolysis, wherein the adding amount of the compound enzyme is 3% of the mass of the fresh houttuynia cordata, dissolving the enzyme into water, the adding amount of the water is 25% of the mass of the fresh houttuynia cordata, then uniformly mixing the enzyme solution and the houttuynia cordata, wherein the enzymolysis temperature is 50 ℃, the enzymolysis pH is 5.5, and the enzymolysis time is 2 hours;
(3) drying the houttuynia cordata after enzymolysis in a freeze dryer at the temperature of minus 40 ℃ for 24 hours;
(4) pulverizing the freeze-dried herba Houttuyniae in a pulverizer, and sieving with a 40 mesh sieve;
(5) placing 100g of herba Houttuyniae powder in supercritical CO 2 Extracting in an extraction kettle by supercritical CO 2 When extracting herba Houttuyniae, the extraction temperature is 40 deg.C, the extraction pressure is 30Mpa, the extraction time is 3 hr, and CO is added 2 The flow rate is 30L/h, volatile oil rich in houttuynin is obtained by separation in a separation kettle, the pressure of the separation kettle is 7MPa, and the temperature of the separation kettle is 50 ℃.
Example 2
Complex enzyme-assisted supercritical CO 2 The method for extracting the houttuynine sodium bisulfite comprises the following steps:
(1) cleaning fresh houttuynia cordata with drinking water, airing the fresh houttuynia cordata in a cool environment to the surface, and cutting into sections with the length of 1-5 mm;
(2) adding a compound enzyme into the cut fresh houttuynia cordata for enzymolysis, wherein the adding amount of the compound enzyme is 2% of the mass of the fresh houttuynia cordata, dissolving the enzyme into water, the adding amount of the water is 30% of the mass of the fresh houttuynia cordata, then uniformly mixing the enzyme solution and the houttuynia cordata, carrying out enzymolysis at 45 ℃, and keeping the enzymolysis pH at 4.5 for 2 hours;
(3) drying the houttuynia cordata after enzymolysis in a freeze dryer at the temperature of minus 30 ℃ for 18 h;
(4) pulverizing the freeze-dried herba Houttuyniae in a pulverizer, and sieving with a 40 mesh sieve;
(5) placing 100g herba Houttuyniae powder in supercritical CO 2 Extracting in an extraction kettle by supercritical CO 2 When extracting herba Houttuyniae, the extraction temperature is 45 deg.C, the extraction pressure is 20Mpa, the extraction time is 2 hr, and CO is added 2 The flow is 25L/h, volatile oil rich in houttuynin is obtained by separation in a separation kettle, the pressure of the separation kettle is 6MPa, and the temperature of the separation kettle is 45 ℃.
Example 3
(1) Cleaning fresh houttuynia cordata with drinking water, airing the fresh houttuynia cordata in a cool environment to the surface, and cutting into sections with the length of 1-5 mm;
(2) adding a compound enzyme into the cut fresh houttuynia cordata for enzymolysis, wherein the adding amount of the compound enzyme is 1% of the mass of the fresh houttuynia cordata, dissolving the enzyme into water, the adding amount of the water is 20% of the mass of the fresh houttuynia cordata, then uniformly mixing the enzyme solution and the houttuynia cordata, wherein the enzymolysis temperature is 50 ℃, the enzymolysis pH is 5.0, and the enzymolysis time is 3 hours;
(3) drying the herba Houttuyniae with the enzymolysis in a freeze-drying machine at-20 deg.C for 12 hr;
(4) pulverizing the freeze-dried herba Houttuyniae in a pulverizer, and sieving with a 40 mesh sieve;
(5) placing 100g herba Houttuyniae powder in supercritical CO 2 Extracting in an extraction kettle by supercritical CO 2 When extracting herba Houttuyniae, the extraction temperature is 50 deg.C, the extraction pressure is 15Mpa, the extraction time is 1h, and CO is added 2 The flow rate is 20L/h, volatile oil rich in houttuynin is obtained by separation in a separation kettle, the pressure of the separation kettle is 5MPa, and the temperature of the separation kettle is 50 ℃.
Example 4
Complex enzyme-assisted supercritical CO 2 The method for extracting the houttuynine sodium bisulfite comprises the following steps:
(1) cleaning fresh houttuynia cordata with drinking water, airing the fresh houttuynia cordata in a cool environment to the surface, and cutting into sections with the length of 1-5 mm;
(2) adding a compound enzyme into the cut fresh houttuynia cordata for enzymolysis, wherein the adding amount of the compound enzyme is 2% of the mass of the fresh houttuynia cordata, dissolving the enzyme into water, the adding amount of the water is 25% of the mass of the fresh houttuynia cordata, then uniformly mixing the enzyme solution and the houttuynia cordata, wherein the enzymolysis temperature is 50 ℃, the enzymolysis pH is 6.5, and the enzymolysis time is 2 hours;
(3) drying the houttuynia cordata after enzymolysis in a freeze dryer at the temperature of minus 30 ℃ for 18 h;
(4) pulverizing the freeze-dried herba Houttuyniae in a pulverizer, and sieving with a 40 mesh sieve;
(5) placing 100g herba Houttuyniae powder in supercritical CO 2 Extracting in an extraction kettleSupercritical CO 2 When extracting herba Houttuyniae, the extraction temperature is 50 deg.C, the extraction pressure is 20Mpa, the extraction time is 2 hr, and CO is added 2 The flow rate is 20L/h, volatile oil rich in houttuynin is obtained by separation in a separation kettle, the pressure of the separation kettle is 6MPa, and the temperature of the separation kettle is 50 ℃.
Comparative example 1
Complex enzyme-assisted supercritical CO 2 The method for extracting the houttuynine sodium bisulfite comprises the following steps: (in comparison with example 3, drying houttuynia cordata with hot air.)
(1) Cleaning fresh houttuynia cordata with drinking water, airing the fresh houttuynia cordata in a cool environment to the surface, and cutting into sections with the length of 1-5 mm;
(2) adding compound enzyme into fresh herba Houttuyniae after cutting for enzymolysis, dissolving enzyme in water with the addition of 3% of the fresh herba Houttuyniae mass, and mixing enzyme solution and herba Houttuyniae uniformly at 50 deg.C and pH of 5.5 for 2 hr
(3) Drying the houttuynia cordata after enzymolysis in a drying machine at the hot air drying temperature of 50 ℃ for 12 h;
(4) pulverizing the freeze-dried herba Houttuyniae in a pulverizer, and sieving with a 40-mesh sieve;
(5) placing 100g of herba Houttuyniae powder in supercritical CO 2 Extracting in an extraction kettle by supercritical CO 2 When extracting herba Houttuyniae, the extraction temperature is 40 deg.C, the extraction pressure is 30Mpa, the extraction time is 3 hr, and CO is added 2 The flow rate is 30L/h, volatile oil rich in houttuynin is obtained by separation in a separation kettle, the pressure of the separation kettle is 7MPa, and the temperature of the separation kettle is 50 ℃.
Comparative example 2
Supercritical CO 2 The method for extracting the houttuynine sodium bisulfite comprises the following steps: (comparison with example 2, without addition of enzyme.)
(1) Cleaning fresh houttuynia cordata with drinking water, airing the fresh houttuynia cordata in a cool environment to the surface, and cutting into sections with the length of 1-5 mm;
(2) carrying out enzymolysis on the cut fresh houttuynia cordata without adding a compound enzyme, and uniformly mixing water and the houttuynia cordata, wherein the addition amount of the water is 30% of the mass of the fresh houttuynia cordata, the enzymolysis temperature is 45 ℃, the enzymolysis pH is 4.5, and the enzymolysis time is 2 hours;
(3) drying the houttuynia cordata after enzymolysis in a freeze dryer at the temperature of minus 30 ℃ for 18 h;
(4) pulverizing the freeze-dried herba Houttuyniae in a pulverizer, and sieving with a 40 mesh sieve;
(5) placing 100g herba Houttuyniae powder in supercritical CO 2 Extracting in an extraction kettle by supercritical CO 2 Extracting herba Houttuyniae with CO at 45 deg.C under 20Mpa for 2 hr 2 The flow is 25L/h, volatile oil rich in houttuynin is obtained by separation in a separation kettle, the pressure of the separation kettle is 6MPa, and the temperature of the separation kettle is 45 ℃.
Comparative example 3
A method for extracting houttuynine sodium bisulfite by organic solvent comprises the following steps: (comparison with example 1, extraction with ethanol)
(1) Cleaning fresh houttuynia cordata with drinking water, airing the fresh houttuynia cordata in a cool environment to the surface, and cutting the fresh houttuynia cordata into sections with the lengths of 1-5 mm;
(2) adding a compound enzyme into fresh houttuynia cordata for enzymolysis, wherein the adding amount of the compound enzyme is 1% of the mass of the fresh houttuynia cordata, dissolving the enzyme into the compound enzyme, the adding amount of water is 20% of the mass of the fresh houttuynia cordata, then uniformly mixing an enzyme solution and the houttuynia cordata, wherein the enzymolysis temperature is 50 ℃, the enzymolysis pH is 5.0, and the enzymolysis time is 3 hours;
(3) drying the herba Houttuyniae after enzymolysis in a freeze dryer at-20 deg.C for 12 hr;
(4) pulverizing the freeze-dried herba Houttuyniae in a pulverizer, and sieving with a 40 mesh sieve;
(5) extracting 100g of houttuynia cordata powder with 95% ethanol for 12 hours, wherein the material ratio is 1: 10. leaching at 40 deg.C for 8 hr, removing ethanol with rotary evaporator, and removing water with anhydrous sodium sulfate to obtain the final product.
Comparative example 4
A method for extracting houttuynin with the assistance of complex enzyme comprises the following steps: (extraction of Houttuynin by steam distillation compared with example 4.)
(1) Cleaning fresh houttuynia cordata with drinking water, airing the fresh houttuynia cordata in a cool environment to the surface, and cutting into sections with the length of 1-5 mm;
(2) adding a compound enzyme into the cut fresh houttuynia cordata for enzymolysis, wherein the adding amount of the compound enzyme is 2% of the mass of the fresh houttuynia cordata, dissolving the enzyme into water, the adding amount of the water is 25% of the mass of the fresh houttuynia cordata, then uniformly mixing the enzyme solution and the houttuynia cordata, wherein the enzymolysis temperature is 50 ℃, the enzymolysis pH is 6.5, and the enzymolysis time is 2 hours;
(3) drying the houttuynia cordata after enzymolysis in a freeze dryer at the temperature of minus 30 ℃ for 18 h;
(4) pulverizing the freeze-dried herba Houttuyniae in a pulverizer, and sieving with a 40 mesh sieve;
(5) 100g of houttuynia cordata powder is put into a 2000mL round-bottom flask, the material-liquid ratio is 1: 10 (g/g), the mixture is soaked for 10 hours, the heating reflux is carried out for 10 hours, and the obtained light yellow volatile oil is collected by steam distillation.
Test example 1
The results of comparing the volatile oil extraction rate and the houttuynin content in the examples and comparative examples are shown in table 1:
TABLE 1 comparison of the extraction rate of volatile oil and the content of houttuynia cordata obtained by different extraction methods
Method Herba Houttuyniae volatile oil extraction ratio% Content of houttuynin/%
Example 1 2.10% 0.15%
Example 2 1.98% 0.10%
Example 3 1.80% 0.08%
Example 4 2.00% 0.12%
Comparative example1 1.70% 0.06%
Comparative example 2 1.75% 0.03%
Comparative example 3 0.12% 0.01%
Comparative example 4 0.04% ND
ND: not detected out
From the experimental results of table 1, it can be found that: the average extraction rates of the volatile oil and the houttuynine sodium bisulfite extracted by the method of the invention are 1.97% and 0.1125% respectively in the products of examples 1-4, 0.9025% and 0.025% respectively in the products of comparative examples 1-4, 2.18 times of the average extraction rate of the volatile oil in the products of comparative examples 1-4, and 4.5 times of the average extraction rate of the volatile oil in the products of comparative examples 1-4. Therefore, the result shows that the method for extracting houttuynine sodium bisulfite with the assistance of the complex enzyme can obviously improve the extraction rate of the oleoresin, and is an excellent extraction method.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (10)

1. Complex enzyme-assisted supercritical CO 2 The method for extracting the houttuynine sodium bisulfite is characterized in that: the method comprises the following steps:
step 1: removing impurities from fresh herba Houttuyniae, cleaning fresh herba Houttuyniae, air drying, cutting into segments;
step 2: adding compound enzyme into the cut fresh houttuynia cordata for enzymolysis;
and 3, step 3: drying the houttuynia cordata after enzymolysis in a freeze dryer;
and 4, step 4: pulverizing the freeze-dried herba Houttuyniae in a pulverizer;
and 5: pulverizing herba Houttuyniae powder in supercritical CO 2 Extracting in an extraction kettle, and separating in a separation kettle to obtain volatile oil rich in houttuynin.
2. The complex enzyme-assisted supercritical CO according to claim 1 2 The method for extracting the houttuynine sodium bisulfite is characterized in that: and (2) cleaning the fresh houttuynia cordata by using drinking water in the step 1, placing the cleaned fresh houttuynia cordata in a cool environment until the surface of the fresh houttuynia cordata is dried, and cutting the fresh houttuynia cordata into sections with the lengths of 1-5 mm.
3. The complex enzyme-assisted supercritical CO according to claim 1 2 The method for extracting the houttuynine sodium bisulfite is characterized in that: in the step 2, the addition amount of the complex enzyme is 1-3% of the mass of the fresh houttuynia cordata.
4. The complex enzyme-assisted supercritical CO according to claim 3 2 The method for extracting the houttuynine sodium bisulfite is characterized in that: the complex enzyme in the step 2 consists of cellulase and pectinase according to the mass ratio of 1: 1.
5. The complex enzyme-assisted supercritical CO according to claim 1 2 The method for extracting the houttuynine sodium bisulfite is characterized in that: in the step 2, the enzymolysis temperature is 40-50 ℃, the enzymolysis pH is 4.5-6.5, and the enzymolysis time is 1-3 h.
6. Compound enzyme assisted supercritical CO according to claim 1 2 The method for extracting the houttuynine sodium bisulfite is characterized in that: and in the step 2, the pH value of enzymolysis is adjusted by using 10mg/ml citric acid.
7. The complex enzyme-assisted supercritical CO according to claim 1 2 The method for extracting the houttuynine sodium bisulfite is characterized in thatThe method comprises the following steps: and (3) drying the houttuynia cordata in the step 3 in a freeze dryer at the temperature of-20 to-40 ℃ for 12 to 24 hours.
8. Compound enzyme assisted supercritical CO according to claim 1 2 The method for extracting the houttuynine sodium bisulfite is characterized in that: and (4) sieving the crushed cordate houttuynia in the step (4) by using a 40-mesh sieve.
9. The complex enzyme-assisted supercritical CO according to claim 1 2 The method for extracting the houttuynine sodium bisulfite is characterized in that: supercritical CO in said step 5 2 When the houttuynia cordata is extracted, the extraction temperature is 40-50 ℃, the extraction pressure is 15-30 Mpa, the extraction time is 1-3 h, and CO is added 2 The flow rate is 20-30L/h.
10. The complex enzyme-assisted supercritical CO according to claim 1 2 The method for extracting the houttuynine sodium bisulfite is characterized in that: the addition amount of the freeze-dried houttuynia cordata powder added into the extraction kettle in the step 5 is 100-200 g, the pressure of the separation kettle is 5-7 MPa, and the temperature of the separation kettle is 40-50 ℃.
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Citations (3)

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