CN106608822B - Method for extracting chlorogenic acid from Dendranthema indicum - Google Patents
Method for extracting chlorogenic acid from Dendranthema indicum Download PDFInfo
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- CN106608822B CN106608822B CN201510702778.1A CN201510702778A CN106608822B CN 106608822 B CN106608822 B CN 106608822B CN 201510702778 A CN201510702778 A CN 201510702778A CN 106608822 B CN106608822 B CN 106608822B
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- ethanol
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- chrysanthemum
- lafeng
- chlorogenic acid
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- PCMORTLOPMLEFB-UHFFFAOYSA-N sinapinic acid Natural products COC1=CC(C=CC(O)=O)=CC(OC)=C1O PCMORTLOPMLEFB-UHFFFAOYSA-N 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 150000003431 steroids Chemical class 0.000 description 1
- QFVOYBUQQBFCRH-VQSWZGCSSA-N steviol Chemical compound C([C@@]1(O)C(=C)C[C@@]2(C1)CC1)C[C@H]2[C@@]2(C)[C@H]1[C@](C)(C(O)=O)CCC2 QFVOYBUQQBFCRH-VQSWZGCSSA-N 0.000 description 1
- 229940032084 steviol Drugs 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 210000004291 uterus Anatomy 0.000 description 1
- 235000019155 vitamin A Nutrition 0.000 description 1
- 239000011719 vitamin A Substances 0.000 description 1
- 235000010374 vitamin B1 Nutrition 0.000 description 1
- 239000011691 vitamin B1 Substances 0.000 description 1
- 235000019164 vitamin B2 Nutrition 0.000 description 1
- 239000011716 vitamin B2 Substances 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Seasonings (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to a method for extracting chlorogenic acid from saussurea involucrate. The method comprises the following steps: A. carrying out enzymolysis; B. alcohol leaching; C. microwave extraction; D. filtering; E. concentrating; F. and (6) cooling. The method for extracting chlorogenic acid from the chrysanthemum indicum has low requirements on process conditions and reasonable process; the extraction process is original, is suitable for industrial production conditions, has high extraction efficiency, simple equipment, low manufacturing cost and easy popularization and application.
Description
Technical Field
The invention relates to a method for extracting chlorogenic acid from saussurea involucrate.
Background
Chlorogenic acid with molecular weight of 354.31, density of 1.65g/cm3, melting point of 205-.
Chlorogenic acid has a wide range of antibacterial effects, but can be inactivated by proteins in vivo. Similar to caffeic acid, the composition can improve central excitability of rat when administered orally or via intraperitoneal injection. Can increase the small intestinal peristalsis of rats and mice and the tension of the uterus of rats. Has choleretic effect and can promote bile secretion of rat. Has sensitizing effect on human, and can cause asthma and dermatitis after inhaling plant dust containing the product.
Chlorogenic acid (Chlorogenic acid), a depside generated from Caffeic acid (Caffeic acid) and Quinic acid (Quinic acid, 1-hydroxyhexahydrogallic acid), is a phenylpropanoid compound generated by plants through the shikimic acid pathway during aerobic respiration.
Chlorogenic acid has wide bioactivity, and the research on the bioactivity of chlorogenic acid in modern science has been deeply carried out in various fields of food, health care, medicine, daily chemical industry and the like. Chlorogenic acid is an important bioactive substance, and has antibacterial, antiviral, leukocyte increasing, liver protecting, gallbladder promoting, antitumor, blood pressure lowering, blood lipid reducing, free radical scavenging, and central nervous system exciting effects.
The Dendranthema indicum is a dry capitate inflorescence of Dendranthema indicum Dendranthemum aidic um E (L1) DesMonl1 var1 aromitum Q1H1L1 iut 1S1E 1Zhang of Compositae, a dry capitate inflorescence of var1 nov1, which is produced in North Hu China Dendrome area, is distributed in a sunny open field with the altitude of more than 2000 meters, is a new variety of Dendranthema, and the whole plant has special strong fragrance, and a Dendranthema indicum sample is collected from North Hu China Dendranthema 10 months in 2004, and is identified as a dry capitate of Dendranthema indicum Dendranthemum a indiicum (L1) DesMonl1 var1 aromitum Q1H1 Liu et S1E 1Zhang of Compositae by the Chinese medicine identification of the university institute of North Ministribunda Dendranthema indicum.
Shanxi mountain area uses Dendranthema indicum for preventing and treating common cold, headache, bacillary dysentery, enteritis, constipation, coronary heart disease, hypertension, etc. The essential oil or extract can be used in medicine, beverage, cigarette and cosmetics. Lujinqing, Hejun, Kingguliang and the like have studied the chemical components of the dried flower essential oil of Dendranthema indicum and identified a plurality of terpenoid compounds; the Gong Fu Jun et al separates and identifies the compounds of robinin, palmitic acid, lauric acid, daucosterol, robinin 2 rhamnoside, chlorogenic acid 272O2 beta 2 glucoside, chlorogenic acid and the like from the Dendranthema indicum.
The shenlongxiangju as a flower variety with characteristics in western and Hui mountain areas is not generally planted in China, and the production place is mainly concentrated in a few places of Shennong shelves and Enshi. Enriches, which are historically important planting areas of chamomile, have a planting tradition for many years, especially have large-area planting in the mountainous area of the Badong, and chamomile is now one of the main local characteristic flower varieties.
The Laifengsheng spices company tries to plant the Dendranthema indicum from 2012, successfully plants the Dendranthema indicum in the low-altitude area with the altitude of 600-1000 meters by using the unique bud sprouting technology, the organic fertilizer rapid-growing technology, the intermittent land culture and other planting technologies, and has bright color, fresh and sweet fragrance, large and uniform heads of the Chrysanthemum, high yield and high medicinal value. The fragrant chrysanthemum planted by Tengsheng spice company has a certain difference with shenlong fragrant chrysanthemum in fragrance characteristics, taste and application value, and becomes the Laifeng fragrant chrysanthemum with own characteristics.
The technology focuses on the 'Laifeng fragrant chrysanthemum' planted in the Laifeng area as a raw material, and aims at the characteristics that the unique fresh and sweet fragrant components of the 'Laifeng fragrant chrysanthemum' are volatile and easy to change and the like, and the modern non-intense heat technical means such as microwave radiation, biological enzyme treatment and the like, the key technical research of high-valued and industrialized key technology of the 'Laifeng fragrant chrysanthemum' is deeply developed from the two aspects of gradient preparation of the whole flavor components and fingerprint identification of the whole flavor components of the 'Laifeng fragrant chrysanthemum', the characteristic fragrant product of the 'Laifeng fragrant chrysanthemum' with high added value is developed, and the industrial production and popularization and application are realized, the transformation from pure fresh food and simple processed products to high-added-value finished products of the Laifeng fragrant chrysanthemum is realized, the commodity value of the Laifeng fragrant chrysanthemum is improved, the industrial chain of the Laifeng fragrant chrysanthemum is driven to extend, the income of farmers is increased, the product market lag in fields is reduced, the agricultural economic benefit is increased, and the high-valued utilization level of local characteristic agricultural and sideline product resources is improved. Meanwhile, the special products with obvious characteristics in the area are pushed to the whole country and the whole world through the deep-processed products of the Laifeng fragrant chrysanthemum.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for extracting chlorogenic acid from fragrant chrysanthemum.
The technical scheme of the invention is as follows: a method for extracting chlorogenic acid from Dendranthema indicum is characterized by comprising the following steps:
A. enzymolysis
Adding Laurencia procumbens, water, cellulase, xylanase, B-glucanase and pectinase into an extraction tank; the adding amount of water is 1-10 times of the weight of the Lafeng fragrant chrysanthemum, and the adding amount of auxiliary materials is the percentage of the weight of the Lafeng fragrant chrysanthemum: 0.1-1% of cellulase, 0.1-1% of xylanase, 0.3-3% of B-glucanase and 0.3-3% of pectinase; controlling the enzymolysis temperature to be 35-55 ℃, starting stirring, and carrying out enzymolysis for: 1-5 hours;
B. alcohol leaching
Adding ethanol with the weight 5-12 times of that of the Lafeng chrysanthemum into an extraction tank, and soaking for 2-24 hours;
C. microwave extraction
Controlling the temperature of the extraction tank to be 50-95 ℃, and extracting for 1-3 hours under the condition that the microwave power is 100-;
D. filtration
Filtering with 100-filter 300-mesh filter bag to obtain filtrate, storing in a storage tank, adding 3-8 times of ethanol into the filter residue, extracting in an extraction tank for 2-6 hr, filtering with 100-filter 300-mesh filter bag to obtain filtrate, mixing the filtrate with the storage tank, and storing;
E. concentrating
Standing the filtrate for 6-24 hr, concentrating in a concentrator at 60-70 deg.C under vacuum degree of 0.8-0.95, and stopping when dry matter content is greater than 55%;
F. cooling down
Cooling the materials to normal temperature to obtain chlorogenic acid extract with solid matter content of more than 55%.
The invention relates to a method for extracting chlorogenic acid from chrysanthemum indicum, which is characterized by comprising the following steps:
A. enzymolysis
Adding Laurencia procumbens, water, cellulase, xylanase, B-glucanase and pectinase into an extraction tank; the adding amount of water is 1-10 times of the weight of the Lafeng fragrant chrysanthemum, and the adding amount of auxiliary materials is the percentage of the weight of the Lafeng fragrant chrysanthemum: 0.1-1% of cellulase, 0.1-1% of xylanase, 0.3-3% of B-glucanase and 0.3-3% of pectinase; controlling the enzymolysis temperature to be 35-55 ℃, starting stirring, and carrying out enzymolysis for: 1-5 hours;
B. alcohol leaching
Adding ethanol with the weight 5-12 times of that of the Lafeng chrysanthemum into an extraction tank, and soaking for 2-24 hours;
C. microwave extraction
Controlling the temperature of the extraction tank to be 50-95 ℃, and extracting for 1-3 hours under the condition that the microwave power is 100-; the microwave extraction system used: adopting a maet-6 microwave extraction system produced by Shanghai Jingqiao drying equipment factory;
D. filtration
Filtering with 100-filter 300-mesh filter bag to obtain filtrate, storing in a storage tank, adding 3-8 times of ethanol into the filter residue, extracting in an extraction tank for 2-6 hr, filtering with 100-filter 300-mesh filter bag to obtain filtrate, mixing the filtrate with the storage tank, and storing;
E. concentrating
Standing the filtrate for 6-24 hr, concentrating in a concentrator at 60-70 deg.C under vacuum degree of 0.8-0.95, recovering ethanol, and stopping ethanol recovery when the concentrated solution is detected by a hammermieter and contains no ethanol; then continuing to evaporate water until the dry matter content of the material is more than 55 percent;
F. cooling down
Cooling the materials to normal temperature to obtain chlorogenic acid extract with solid matter content of more than 55%.
The invention relates to a method for extracting chlorogenic acid from Laifeng fragrant chrysanthemum, wherein the main chemical components of Laifeng fragrant chrysanthemum are researched, the main components of Laifeng fragrant chrysanthemum comprise chlorogenic acid, luteolin, linarin, amino acids, polysaccharides, flavonoids, chlorogenic acid, volatile essential oil and the like, the volatile components of Laifeng fragrant chrysanthemum are measured, and the contents of total flavonoids and volatile oil of different chrysanthemums are compared, and the results show that the contents of the total flavonoids and the volatile oil of Laifeng fragrant chrysanthemum are higher, the volatile oil comprises cis-linalool oxide (21.84%), steviol (4.25%), elemene (8.23%), linalool (13.90%), 2, 3-butanediol (5.69%), only-phellandrene (31.05%), p-cymene (38.08%), linalool oxide (7.63%), and linalool oxide (29.38%); the basic components of the dry Laifeng fragrant chrysanthemum are as follows: 80-90% of dry matter, 1-1.8% of protein, 6.3-10.8% of carbohydrate, 0.6-1.7% of crude fiber, 0.1% of fat, 0.2-0.5% of calcium, 0.05% of phosphorus, abundant vitamins A, B1, B2 and C and trace mineral elements such as iron, potassium, manganese, zinc and the like. The Laifeng fragrant chrysanthemum contains about 0.015 percent (dry content is about 0.15 percent) of volatile oil and mainly aromatic compounds, and although the content of the volatile oil is small, the compounds form the specific flavor and physiological functional components of the Laifeng fragrant chrysanthemum, and the method is one of the focuses of the current research on the physiological active components of the Laifeng fragrant chrysanthemum. The main functional components of the Laifeng fragrant chrysanthemum can be divided into the following categories:
antioxidant activity. Chlorogenic acid and luteolin are main components in the Laifeng fragrant chrysanthemum, and have stronger oxidation resistance; flavonoid compounds mainly present in leaves, stems and outer skins, represented by flavonoids, flavonols and anthocyans; phenylpropanoid phenolic compounds mainly existing in leaves and stems, including caffeic acid, ferulic acid, sinapic acid and other monomers and derivatives thereof; steroids and nitrogen-containing compounds.
The Laifeng fragrant chrysanthemum has special physiological function characteristics, the deep-processed products of the Laifeng fragrant chrysanthemum and the Laifeng fragrant chrysanthemum have the effects of sterilizing and diminishing inflammation, calming the liver and improving eyesight, and dispelling wind and reducing blood pressure, and the Laifeng fragrant chrysanthemum is used for preventing and treating diseases such as cold, headache, bacillary dysentery, enteritis, constipation, coronary heart disease, hypertension and the like in western Hubei mountainous areas.
The method for extracting chlorogenic acid from the chrysanthemum indicum has low requirements on process conditions and reasonable process; the extraction process is original, is suitable for industrial production conditions, has high extraction efficiency, simple equipment, low manufacturing cost and easy popularization and application.
The raw materials and equipment used in the method are common and common raw materials and equipment, so that the dependence on expensive raw materials and instruments in the industrial production process is avoided, and the production cost is greatly reduced; the Laifeng fragrant chrysanthemum is easy to plant, can be used for both cuttage and tissue culture, has high yield and moderate cost, is convenient to source, and ensures subsequent resources. The application of the Lafeng fragrant chrysanthemum as the raw material not only greatly improves the utilization efficiency of the Lafeng fragrant chrysanthemum winter and the added value of the Lafeng fragrant chrysanthemum, but also gets rid of the dependence on other materials such as the raw materials of the luteolin and the peanut shell, can relieve the large demand of the market on other raw materials, and simultaneously can fully utilize the abandoned Lafeng fragrant chrysanthemum and protect the plant resources such as the luteolin.
The method has simple operation, does not need resin chromatography filtration technology, does not need precise instruments or automatic equipment, and can be used for production in village and town enterprises with abundant Laifeng chrysanthemum resources, thereby greatly reducing the production cost of chlorogenic acid and simplifying the production process.
The reagents used in the invention are all nontoxic, cheap and mass-produced chemical reagents, and mature conventional technology for recovering the reagents can be utilized in the whole process, so that the emission of wastes to the environment is greatly reduced.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1: the invention relates to a method for extracting chlorogenic acid from chrysanthemum indicum, which comprises the following steps:
A. enzymolysis
Adding Laurencia procumbens, water, cellulase, xylanase, B-glucanase and pectinase into an extraction tank; the adding amount of water is 1 time of the weight of the Lafeng fragrant chrysanthemum, and the adding amount of auxiliary materials is the percentage of the weight of the Lafeng fragrant chrysanthemum: 0.1% of cellulase, 0.1% of xylanase, 0.3% of B-glucanase and 0.3% of pectinase; controlling the enzymolysis temperature to be 35 ℃, starting stirring, and carrying out enzymolysis for: 1 hour;
B. alcohol leaching
Adding ethanol which is 5 times of the weight of the Lafeng fragrant chrysanthemum into an extraction tank, and soaking for 2 hours;
C. microwave extraction
Extracting for 1 hour under the conditions that the temperature of the extracting tank is controlled to be 50 ℃ and the microwave power is 100 kw; the microwave extraction system used: adopting a maet-6 microwave extraction system produced by Shanghai Jingqiao drying equipment factory;
D. filtration
Filtering with 100 mesh filter bag to obtain filtrate, storing in storage tank, adding 3 times of ethanol into the residue, extracting in extraction tank for 2 hr, filtering with 100 mesh filter bag to obtain filtrate, mixing filtrates, and storing in storage tank;
E. concentrating
Standing the filtrate for 6 hr, concentrating in a concentrator at 60 deg.C under vacuum degree of 0.8, recovering ethanol, and recovering ethanol in an ethanol storage tank, wherein the ethanol recovery is stopped when the concentrated solution is detected by a hammerhead alcohol meter and does not contain ethanol; then continuing to evaporate water until the dry matter content of the material is more than 55 percent;
F. cooling down
Cooling the materials to normal temperature to obtain chlorogenic acid extract with solid matter content of more than 55%.
Example 2: the invention relates to a method for extracting chlorogenic acid from chrysanthemum indicum, which comprises the following steps:
A. enzymolysis
Adding Laurencia procumbens, water, cellulase, xylanase, B-glucanase and pectinase into an extraction tank; the adding amount of water is 10 times of the weight of the Lafeng fragrant chrysanthemum, and the adding amount of auxiliary materials is the percentage of the weight of the Lafeng fragrant chrysanthemum: 1% of cellulase, 1% of xylanase, 3% of B-glucanase and 3% of pectinase; controlling the enzymolysis temperature to be 55 ℃, starting stirring, and carrying out enzymolysis for: 5 hours;
B. alcohol leaching
Adding ethanol which is 12 times of the weight of the Lafeng fragrant chrysanthemum into an extraction tank, and soaking for 24 hours;
C. microwave extraction
Controlling the temperature of the extraction tank to be 95 ℃, and extracting for 3 hours under the condition that the microwave power is 500 kw; the microwave extraction system used: adopting a maet-6 microwave extraction system produced by Shanghai Jingqiao drying equipment factory;
D. filtration
Filtering with 300 mesh filter bag to obtain filtrate, storing in storage tank, adding 8 times of ethanol into the residue, extracting in extraction tank for 6 hr, filtering with 300 mesh filter bag to obtain filtrate, mixing filtrates, and storing in storage tank;
E. concentrating
Standing the filtrate for 24 hr, concentrating in a concentrator at 70 deg.C under vacuum degree of 0.95, recovering ethanol, and stopping ethanol recovery when the concentrated solution is detected by a hammerhead alcohol meter and contains no ethanol; then continuing to evaporate water until the dry matter content of the material is more than 55 percent;
F. cooling down
Cooling the materials to normal temperature to obtain chlorogenic acid extract with solid matter content of more than 55%.
Example 3: the invention relates to a method for extracting chlorogenic acid from chrysanthemum indicum, which comprises the following steps:
A. enzymolysis
Adding Laurencia procumbens, water, cellulase, xylanase, B-glucanase and pectinase into an extraction tank; the adding amount of water is 5 times of the weight of the Lafeng fragrant chrysanthemum, and the adding amount of auxiliary materials is the percentage of the weight of the Lafeng fragrant chrysanthemum: 0.5% of cellulase, 0.5% of xylanase, 1.5% of B-glucanase and 1.5% of pectinase; controlling the enzymolysis temperature to be 45 ℃, starting stirring, and carrying out enzymolysis for: 2.5 hours;
B. alcohol leaching
Adding ethanol which is 8 times of the weight of the Lafeng fragrant chrysanthemum into an extraction tank, and soaking for 12 hours;
C. microwave extraction
Controlling the temperature of the extraction tank to be 75 ℃, and extracting for 1.5 hours under the condition that the microwave power is 300 kw; the microwave extraction system used: adopting a maet-6 microwave extraction system produced by Shanghai Jingqiao drying equipment factory;
D. filtration
Filtering with 200 mesh filter bag to obtain filtrate, storing in storage tank, adding 5.5 times of ethanol into the residue, extracting in extraction tank for 4 hr, filtering with 200 mesh filter bag to obtain filtrate, mixing filtrates, and storing in storage tank;
E. concentrating
Standing the filtrate for 15 hr, concentrating in a concentrator at 65 deg.C under vacuum degree of 0.9, recovering ethanol, and recovering ethanol in an ethanol storage tank, wherein the ethanol recovery is stopped when the concentrated solution is detected by a hammerhead alcohol meter and does not contain ethanol; then continuing to evaporate water until the dry matter content of the material is more than 55 percent;
F. cooling down
Cooling the materials to normal temperature to obtain chlorogenic acid extract with solid matter content of more than 55%.
Example 4: the invention relates to a method for extracting chlorogenic acid from chrysanthemum indicum, which comprises the following steps:
A. enzymolysis
Adding Laurencia procumbens, water, cellulase, xylanase, B-glucanase and pectinase into an extraction tank; the adding amount of water is 8 times of the weight of the Lafeng fragrant chrysanthemum, and the adding amount of auxiliary materials is the percentage of the weight of the Lafeng fragrant chrysanthemum: 0.8% of cellulase, 0.8% of xylanase, 2% of B-glucanase and 2% of pectinase; controlling the enzymolysis temperature to be 50 ℃, starting stirring, and carrying out enzymolysis for: 4 hours;
B. alcohol leaching
Adding ethanol which is 10 times of the weight of the Lafeng fragrant chrysanthemum into an extraction tank, and soaking for 20 hours;
C. microwave extraction
Controlling the temperature of the extraction tank to be 80 ℃, and extracting for 2 hours under the condition that the microwave power is 400 kw; the microwave extraction system used: adopting a maet-6 microwave extraction system produced by Shanghai Jingqiao drying equipment factory;
D. filtration
Filtering with 250 mesh filter bag to obtain filtrate, storing in storage tank, adding 7 times of ethanol into the residue, extracting in extraction tank for 5 hr, filtering with 250 mesh filter bag to obtain filtrate, mixing filtrates, and storing in storage tank;
E. concentrating
Standing the filtrate for 20 hr, concentrating in a concentrator at 68 deg.C under vacuum degree of 0.92, recovering ethanol, and recovering ethanol to an ethanol storage tank, wherein when the concentrated solution is detected by a hammerhead alcohol meter and contains no ethanol, the ethanol recovery is stopped; then continuing to evaporate water until the dry matter content of the material is more than 55 percent;
F. cooling down
Cooling the materials to normal temperature to obtain chlorogenic acid extract with solid matter content of more than 55%.
Example 5: the invention relates to a method for extracting chlorogenic acid from chrysanthemum indicum, which comprises the following steps:
A. enzymolysis
Adding Laurencia procumbens, water, cellulase, xylanase, B-glucanase and pectinase into an extraction tank; the adding amount of water is 4 times of the weight of the Lafeng fragrant chrysanthemum, and the adding amount of auxiliary materials is the percentage of the weight of the Lafeng fragrant chrysanthemum: 0.4% of cellulase, 0.4% of xylanase, 1% of B-glucanase and 1% of pectinase; controlling the enzymolysis temperature to be 38 ℃, starting stirring, and carrying out enzymolysis for: 2 hours;
B. alcohol leaching
Adding ethanol which is 8 times of the weight of the Lafeng fragrant chrysanthemum into an extraction tank, and soaking for 5 hours;
C. microwave extraction
Controlling the temperature of the extraction tank to be 70 ℃, and extracting for 1.2 hours under the condition that the microwave power is 150 kw; the microwave extraction system used: adopting a maet-6 microwave extraction system produced by Shanghai Jingqiao drying equipment factory;
D. filtration
Filtering with 150 mesh filter bag to obtain filtrate, storing in storage tank, adding 4 times of ethanol into the residue, extracting in extraction tank for 3 hr, filtering with 150 mesh filter bag to obtain filtrate, mixing filtrates, and storing in storage tank;
E. concentrating
Standing the filtrate for 8 hr, concentrating in a concentrator at 68 deg.C under vacuum degree of 0.85, recovering ethanol, and stopping ethanol recovery when the concentrated solution is detected by a hammerhead alcohol meter and contains no ethanol; then continuing to evaporate water until the dry matter content of the material is more than 55 percent;
F. cooling down
Cooling the materials to normal temperature to obtain chlorogenic acid extract with solid matter content of more than 55%.
Example 6: the invention relates to a method for extracting chlorogenic acid from chrysanthemum indicum, which comprises the following steps:
A. enzymolysis
Adding Laurencia procumbens, water, cellulase, xylanase, B-glucanase and pectinase into an extraction tank; the adding amount of water is 6 times of the weight of the Lafeng fragrant chrysanthemum, and the adding amount of auxiliary materials is the percentage of the weight of the Lafeng fragrant chrysanthemum: 0.6% of cellulase, 0.6% of xylanase, 2.1% of B-glucanase and 2.1% of pectinase; controlling the enzymolysis temperature to be 39 ℃, starting stirring, and carrying out enzymolysis for: 4 hours;
B. alcohol leaching
Adding ethanol which is 7 times of the weight of the Lafeng fragrant chrysanthemum into an extraction tank, and soaking for 20 hours;
C. microwave extraction
Controlling the temperature of the extraction tank to be 80 ℃, and extracting for 2.5 hours under the condition that the microwave power is 400 kw; the microwave extraction system used: adopting a maet-6 microwave extraction system produced by Shanghai Jingqiao drying equipment factory;
D. filtration
Filtering with 300 mesh filter bag to obtain filtrate, storing in storage tank, adding 6 times of ethanol into the residue, extracting in extraction tank for 5 hr, filtering with 300 mesh filter bag to obtain filtrate, mixing filtrates, and storing in storage tank;
E. concentrating
Standing the filtrate for 22 hr, concentrating in a concentrator at 66 deg.C under vacuum degree of 0.89, recovering ethanol, and recovering ethanol to an ethanol storage tank, wherein ethanol recovery is stopped when the concentrated solution is detected by a hammerhead alcohol meter and does not contain ethanol; then continuing to evaporate water until the dry matter content of the material is more than 55 percent;
F. cooling down
Cooling the materials to normal temperature to obtain chlorogenic acid extract with solid matter content of more than 55%.
Claims (2)
1. A method for extracting chlorogenic acid from Dendranthema indicum is characterized by comprising the following steps:
A. enzymolysis
Adding Laurencia procumbens, water, cellulase, xylanase, B-glucanase and pectinase into an extraction tank; the adding amount of water is 1-10 times of the weight of the Lafeng fragrant chrysanthemum, and the adding amount of auxiliary materials is the percentage of the weight of the Lafeng fragrant chrysanthemum: 0.1-1% of cellulase, 0.1-1% of xylanase, 0.3-3% of B-glucanase and 0.3-3% of pectinase; controlling the enzymolysis temperature to be 35-55 ℃, starting stirring, and carrying out enzymolysis for: 1-5 hours;
B. alcohol leaching
Adding ethanol with the weight 5-12 times of that of the Lafeng chrysanthemum into an extraction tank, and soaking for 2-24 hours;
C. microwave extraction
Controlling the temperature of the extraction tank to be 50-95 ℃, and extracting for 1-3 hours under the condition that the microwave power is 100-;
D. filtration
Filtering with 100-filter 300-mesh filter bag to obtain filtrate, storing in a storage tank, adding 3-8 times of ethanol into the filter residue, extracting in an extraction tank for 2-6 hr, filtering with 100-filter 300-mesh filter bag to obtain filtrate, mixing the filtrate with the storage tank, and storing;
E. concentrating
Standing the filtrate for 6-24 hr, concentrating in a concentrator at 60-70 deg.C under vacuum degree of 0.8-0.95, and stopping when dry matter content is greater than 55%;
F. cooling down
Cooling the materials to normal temperature to obtain chlorogenic acid extract with solid matter content of more than 55%.
2. The method for extracting chlorogenic acid from saussurea involucrate according to claim 1, comprising the steps of:
A. enzymolysis
Adding Laurencia procumbens, water, cellulase, xylanase, B-glucanase and pectinase into an extraction tank; the adding amount of water is 1-10 times of the weight of the Lafeng fragrant chrysanthemum, and the adding amount of auxiliary materials is the percentage of the weight of the Lafeng fragrant chrysanthemum: 0.1-1% of cellulase, 0.1-1% of xylanase, 0.3-3% of B-glucanase and 0.3-3% of pectinase; controlling the enzymolysis temperature to be 35-55 ℃, starting stirring, and carrying out enzymolysis for: 1-5 hours;
B. alcohol leaching
Adding ethanol with the weight 5-12 times of that of the Lafeng chrysanthemum into an extraction tank, and soaking for 2-24 hours;
C. microwave extraction
Controlling the temperature of the extraction tank to be 50-95 ℃, and extracting for 1-3 hours under the condition that the microwave power is 100-; the microwave extraction system used: adopting a maet-6 microwave extraction system produced by Shanghai Jingqiao drying equipment factory;
D. filtration
Filtering with 100-filter 300-mesh filter bag to obtain filtrate, storing in a storage tank, adding 3-8 times of ethanol into the filter residue, extracting in an extraction tank for 2-6 hr, filtering with 100-filter 300-mesh filter bag to obtain filtrate, mixing the filtrate with the storage tank, and storing;
E. concentrating
Standing the filtrate for 6-24 hr, concentrating in a concentrator at 60-70 deg.C under vacuum degree of 0.8-0.95, recovering ethanol, and stopping ethanol recovery when the concentrated solution is detected by a hammermieter and contains no ethanol; then continuing to evaporate water until the dry matter content of the material is more than 55 percent;
F. cooling down
Cooling the materials to normal temperature to obtain chlorogenic acid extract with solid matter content of more than 55%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006064150A1 (en) * | 2004-12-17 | 2006-06-22 | Laboratoires Elysee | Method for obtaining stabilised natural polyphenols, polyphenols thus obtained, and use of said polyphenols in the metabolism of glucids |
| CN102476996A (en) * | 2010-11-22 | 2012-05-30 | 郭翀 | Extraction process of chlorogenic acid in honeysuckle |
| CN102731309A (en) * | 2012-06-25 | 2012-10-17 | 浙江农林大学 | Method for extracting and separating chlorogenic acid from chrysanthemum indicum |
| CN103012147A (en) * | 2011-09-23 | 2013-04-03 | 盛一诺 | Extraction process of chlorogenic acid in honeysuckle |
| CN103086889A (en) * | 2013-02-22 | 2013-05-08 | 王星敏 | Method for extracting chlorogenic acid from Lonicera japonica leaves activated under catalysis of enzyme |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006064150A1 (en) * | 2004-12-17 | 2006-06-22 | Laboratoires Elysee | Method for obtaining stabilised natural polyphenols, polyphenols thus obtained, and use of said polyphenols in the metabolism of glucids |
| CN102476996A (en) * | 2010-11-22 | 2012-05-30 | 郭翀 | Extraction process of chlorogenic acid in honeysuckle |
| CN103012147A (en) * | 2011-09-23 | 2013-04-03 | 盛一诺 | Extraction process of chlorogenic acid in honeysuckle |
| CN102731309A (en) * | 2012-06-25 | 2012-10-17 | 浙江农林大学 | Method for extracting and separating chlorogenic acid from chrysanthemum indicum |
| CN103086889A (en) * | 2013-02-22 | 2013-05-08 | 王星敏 | Method for extracting chlorogenic acid from Lonicera japonica leaves activated under catalysis of enzyme |
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