CN112245481A - Extraction method of hawthorn leaf extract and hawthorn leaf extract - Google Patents
Extraction method of hawthorn leaf extract and hawthorn leaf extract Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
- A61K36/734—Crataegus (hawthorn)
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The invention relates to the technical field of biological extraction, and particularly relates to a hawthorn leaf extract and an extraction method thereof, wherein the extraction method comprises the following steps: (1) pulverizing folium crataegi into folium crataegi powder, percolating with ethanol as solvent, and collecting percolate; (2) concentrating the percolate under reduced pressure and recovering ethanol to obtain concentrated solution A; (3) adding water to dilute the concentrated solution A; extracting the diluent by adopting petroleum ether, and separating a water layer to obtain a treatment solution; (4) extracting the treatment solution by using ethyl acetate to obtain an extracting solution; (5) concentrating the extracting solution under reduced pressure and recovering ethyl acetate to obtain a concentrated solution B; drying to obtain folium crataegi extract. The extracted hawthorn leaf extract has the total flavone content of more than 90 percent, the hyperin content of more than 0.5 percent and high yield of active ingredients, and the extraction method has simple process, high extraction efficiency, convenient operation and control and contribution to industrial production.
Description
Technical Field
The invention relates to the technical field of biological extraction, and particularly relates to a method for extracting a hawthorn leaf extract.
Background
The folium crataegi is dry leaf of Crataegus pinnatifida (L.) Hassk of Crataegus of Rosaceae, total flavone and hyperoside are effective components extracted from dry leaf of Crataegus pinnatifida (L.) Hassk, and the total flavone has effects of lowering blood pressure, increasing coronary blood flow, reducing blood lipid, tonifying heart, and resisting arrhythmia. Hyperin has good protective effect on myocardial ischemia reperfusion, cerebral infarction, etc. The related preparation is widely used for treating cardiovascular and cerebrovascular diseases, such as Yixintong soft capsule, Yixintong tablet, etc. However, the total flavone content extracted from the hawthorn leaf extract obtained in the prior art does not exceed 80%, and meanwhile, the content of hyperin is not required, or the extracted hyperin content is very low, the extraction method is complex in process, and the existing extraction method of the hawthorn leaf extract needs to be further improved.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the hawthorn leaf extract and the extraction method thereof, wherein the total flavone content in the hawthorn leaf extract extracted by the extraction method is more than 90%, and the hyperin content is more than 0.5%.
The invention is realized by the following technical scheme: a method for extracting hawthorn leaf extract comprises the following steps:
(1) pulverizing folium crataegi into folium crataegi powder, percolating with ethanol as solvent, and collecting percolate;
(2) concentrating the percolate under reduced pressure and recovering ethanol to obtain concentrated solution A;
(3) adding water to dilute the concentrated solution A to obtain a diluted solution; extracting the diluent by adopting petroleum ether, and separating a water layer to obtain a treatment solution;
(4) extracting the treatment solution by using ethyl acetate to obtain an extracting solution;
(5) concentrating the extracting solution under reduced pressure and recovering ethyl acetate to obtain a concentrated solution B; drying to obtain folium crataegi extract.
In the extraction method of the hawthorn leaf extract, ethanol is adopted for percolation, active ingredients in the hawthorn leaf extract are extracted in the percolation process, and a large amount of chlorophyll is dissolved out and is not removed, so that the contents of the active ingredients, namely total flavonoids and hyperin, can be influenced; the invention removes pigment by using a petroleum ether extraction method, extracts the required total flavone and hyperin by using ethyl acetate, and controls the amount of petroleum ether and ethyl acetate; the prepared hawthorn leaf extract has the total flavone content of more than 90 percent and the hyperin content of more than 0.5 percent, and the extraction method has the advantages of high yield of active ingredients, simple extraction process, high extraction efficiency, convenient operation and control, low production cost, contribution to industrial production and high recovery rate of the adopted solvent.
Further, in the step (1), the adding amount of ethanol is 9-11 times of the amount of the hawthorn leaf powder, the concentration of the ethanol is 95% wt, and the percolation speed is 2.5-3.5 mL/min. Namely, 10L of 95% ethanol is added into every kg of hawthorn leaf powder. The hawthorn leaves are firstly coarsely crushed and then are subjected to ultrafine crushing until the hawthorn leaves are sieved by a 180-mesh sieve.
Further, in the step (2), the percolate is subjected to reduced pressure to recover ethanol, and the ethanol is concentrated until the relative density of the concentrated solution A is 1.03-1.05 to obtain the concentrated solution A.
Further, in the step (2), the pressure for the reduced pressure concentration is 300-500 Pa. By adopting the step of reduced pressure concentration, the invention has the advantages of high concentration efficiency, difficult damage of active ingredients, good product quality and improvement.
Further, in the step (3), the volume ratio of the concentrated solution A to the added water is 1:0.9-1.1, and the volume ratio of the diluent to the petroleum ether is 1: 5.5-6.5.
Further, in the step (3), the temperature for extracting by adopting petroleum ether is 65-80 ℃.
The invention adopts the petroleum ether extraction method, strictly controls each process parameter in the extraction process and controls the dosage of each component, is beneficial to removing pigment, improves the purity of the hawthorn leaf extract, has small content loss of active ingredients of total flavonoids and hyperin, and improves the product yield and the extraction efficiency of the active ingredients.
Further, in the step (4), the volume ratio of the treatment solution to the ethyl acetate is 1: 3.8-4.2.
Further, in the step (4), ethyl acetate is adopted to perform ultrasonic extraction on the treatment solution, the power of the ultrasonic extraction is 125-. The invention adopts ethyl acetate to carry out ultrasonic wave interval ultrasonic extraction on the treatment solution, is beneficial to improving the contents of the active ingredients of total flavonoids and hyperin, and has high yield of the active ingredients, simple and easily controlled operation and high extraction efficiency.
Further, in the step (5), the pressure for the reduced pressure concentration is 300-500 Pa. By adopting the step of reduced pressure concentration, the invention has the advantages of high concentration efficiency, difficult damage of active ingredients, high content yield of active ingredients total flavone and hyperin and good product quality.
Further, in the step (5), the concentrated solution B is subjected to vacuum freeze-drying, and the vacuum freeze-drying method includes the following steps:
a1 and the concentrated solution B are pre-frozen after being concentrated to the water content of less than 60 percent, and a pre-frozen extract A1 is obtained, wherein the pre-freezing time is-25 to-20 ℃, and the pre-freezing time is 45 to 75 min;
a2, placing the pre-frozen extract A1 in a vacuum freeze drying device for freezing, wherein the freezing time is-45 to-35 ℃, the vacuum degree is 50 to 100Pa, and the freeze drying time is 90 to 150min, so as to obtain an extract A2;
a3, cooling the temperature in the vacuum freeze drying equipment to-55-50 deg.C, vacuumizing for sublimation drying, keeping the negative pressure for 60-120min when the temperature reaches 28-34 deg.C, pressurizing to normal pressure, and taking out the dried extract for use.
Further, the step a3 is specifically: reducing the temperature in the vacuum freeze drying equipment to-55 to-50 ℃, vacuumizing and carrying out sublimation drying, wherein the temperature rise step is as follows: s1, in the stage process that the temperature is increased from-50 ℃ to-30 ℃, the temperature rising speed is 4-6 ℃/10min, and the vacuum degree is kept at 10-30 Pa; s2, raising the temperature from-30 ℃ to-10 ℃, wherein the temperature raising speed is 4-6 ℃/10min, and the vacuum degree is kept between 35Pa and 55 Pa; s3, in the stage from-10 ℃ to 0 ℃, the temperature rising speed is 7-9 ℃/10min, and the vacuum degree is kept at 60-80 Pa; s4, heating from 0 deg.C to 28-34 deg.C at a heating rate of 7-9 deg.C/10 min, maintaining vacuum degree at 10-30Pa, maintaining negative pressure for 60-120min, pressurizing to normal pressure, and taking out dried extract.
By adopting the vacuum freeze-drying process and matching different heating speeds and vacuum degrees according to different stages, the loss of active ingredients in the hawthorn leaf extract is small, the water content is reduced to be below 4%, the preservation time of the extract can be prolonged, the quality of the product is not influenced, the quality of the product is stable, the purpose of quick sublimation can be achieved, the freeze-drying time is shortened, and the energy consumption can be greatly saved.
The invention also provides a hawthorn leaf extract prepared by the extraction method of the hawthorn leaf extract. In the hawthorn leaf extract, the content of total flavonoids is more than 90 percent, the content of hyperin is more than 0.5 percent, the yield of active ingredients is high, the product purity is high, and the product quality is stable.
The invention has the beneficial effects that: in the extraction method of the hawthorn leaf extract, ethanol is adopted for percolation, active ingredients in the hawthorn leaf extract are extracted in the percolation process, and a large amount of chlorophyll is dissolved out and is not removed, so that the contents of the active ingredients, namely total flavonoids and hyperin, can be influenced; the invention removes pigment by using a petroleum ether extraction method, extracts the required total flavone and hyperin by using ethyl acetate, and controls the amount of petroleum ether and ethyl acetate; the prepared hawthorn leaf extract has the total flavone content of more than 90 percent and the hyperin content of more than 0.5 percent, and the extraction method has the advantages of high yield of active ingredients, simple extraction process, high extraction efficiency, convenient operation and control, low production cost and contribution to industrial production.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
In this embodiment, an extraction method of a hawthorn leaf extract includes the following steps:
(1) pulverizing folium crataegi into folium crataegi powder, percolating with ethanol as solvent, and collecting percolate;
(2) concentrating the percolate under reduced pressure and recovering ethanol to obtain concentrated solution A;
(3) adding water to dilute the concentrated solution A to obtain a diluted solution; extracting the diluent by adopting petroleum ether, and separating a water layer to obtain a treatment solution;
(4) extracting the treatment solution by using ethyl acetate to obtain an extracting solution;
(5) concentrating the extracting solution under reduced pressure and recovering ethyl acetate to obtain a concentrated solution B; drying to obtain folium crataegi extract.
Further, in the step (1), the adding amount of ethanol is 10 times of the amount of the hawthorn leaf powder, the concentration of the ethanol is 95% wt, and the percolation speed is 3 mL/min. Namely, 10L of 95% ethanol is added into every kg of hawthorn leaf powder. The hawthorn leaves are firstly coarsely crushed and then are subjected to ultrafine crushing until the hawthorn leaves are sieved by a 180-mesh sieve.
Further, in the step (2), ethanol is recovered from the percolate under reduced pressure, and the percolate is concentrated until the relative density of the concentrated solution A is 1.04 to obtain the concentrated solution A. The pressure of the reduced pressure concentration is 400 Pa.
Further, in the step (3), the volume ratio of the concentrated solution A to the added water is 1:1, and the volume ratio of the diluent to the petroleum ether is 1:6. The temperature for extraction with petroleum ether was 70 ℃.
Further, in the step (4), the volume ratio of the treatment solution to ethyl acetate is 1:4.
Further, in the step (4), ethyl acetate is adopted to perform ultrasonic extraction on the treatment solution, the power of the ultrasonic extraction is 130w, the ultrasonic frequency is 35kHz, the extraction time is 45min, the ultrasonic extraction adopts interval ultrasonic extraction, the interval time is 75s, and the ultrasonic time is 180s each time.
Further, in the step (5), the pressure of the reduced pressure concentration is 400 Pa.
Further, in the step (5), the concentrated solution B is subjected to vacuum freeze-drying, and the vacuum freeze-drying method includes the following steps:
a1 and the concentrated solution B are concentrated to the water content of less than 60 percent, and then pre-frozen to obtain pre-frozen extract A1, wherein the pre-freezing time is-22 ℃, and the pre-freezing time is 60 min;
a2, freezing the pre-frozen extract A1 in vacuum freeze-drying equipment at-40 deg.C under vacuum degree of 60Pa for 120min to obtain extract A2;
a3, cooling to-52 deg.C, vacuum-pumping for sublimation drying, maintaining negative pressure for 90min when the temperature reaches 30 deg.C, pressurizing to normal pressure, and taking out the dried extract. The water content of the extract is reduced to below 4% after vacuum freeze drying.
Further, the step a3 is specifically: reducing the temperature in the vacuum freeze drying equipment to-52 ℃, vacuumizing and carrying out sublimation drying, wherein the temperature rise step is as follows: s1, in the stage process that the temperature is increased from-50 ℃ to-30 ℃, the temperature rising speed is 5 ℃/10min, and the vacuum degree is kept at 20 Pa; s2, heating from-30 ℃ to-10 ℃, wherein the heating speed is 5 ℃/10min, and the vacuum degree is kept at 40 Pa; s3, in the stage from-10 ℃ to 0 ℃, the temperature rising speed is 8 ℃/10min, and the vacuum degree is kept at 70 Pa; s4, heating from 0 deg.C to 30 deg.C at a heating rate of 8 deg.C/10 min, maintaining vacuum degree at 20Pa, maintaining negative pressure for 90min, slowly pressurizing to normal pressure, and taking out dried extract.
Example 2
In this embodiment, in the step (1), the amount of ethanol added is 9 times of the amount of the hawthorn leaf powder, the concentration of ethanol is 95% wt, and the percolation rate is 2.5 mL/min.
Further, in the step (2), ethanol is recovered from the percolate under reduced pressure, and the percolate is concentrated until the relative density of the concentrated solution A is 1.03 to obtain the concentrated solution A. The pressure of the reduced pressure concentration is 300 Pa.
Further, in the step (3), the volume ratio of the concentrated solution A to the added water is 1:0.9, and the volume ratio of the diluent to the petroleum ether is 1: 5.5. The temperature for extraction with petroleum ether was 65 ℃.
Further, in the step (4), the volume ratio of the treatment solution to ethyl acetate is 1: 3.8.
Further, in the step (4), ethyl acetate is adopted to perform ultrasonic extraction on the treatment solution, the power of the ultrasonic extraction is 125w, the ultrasonic frequency is 30kHz, the extraction time is 30min, the ultrasonic extraction adopts interval ultrasonic extraction, the interval time is 60s, and the ultrasonic time is 150s each time.
Further, in the step (5), the pressure of the reduced pressure concentration is 300 Pa.
Further, in the step (5), the concentrated solution B is subjected to vacuum freeze-drying, and the vacuum freeze-drying method includes the following steps:
a1 and the concentrated solution B are concentrated to water content less than 60%, and then pre-frozen to obtain pre-frozen extract A1, wherein the pre-freezing time is-25 ℃ and the pre-freezing time is 45-75 min;
a2, freezing the pre-frozen extract A1 in vacuum freeze-drying equipment at-45 deg.C under vacuum degree of 50Pa for 90min to obtain extract A2;
a3, cooling to-55 deg.C, vacuum-pumping for sublimation drying, maintaining negative pressure for 120min when the temperature reaches 28 deg.C, pressurizing to normal pressure, and taking out the dried extract.
Further, the step a3 is specifically: reducing the temperature in the vacuum freeze drying equipment to-55 ℃, vacuumizing and carrying out sublimation drying, wherein the temperature rise step is as follows: s1, in the stage process that the temperature is increased from-50 ℃ to-30 ℃, the temperature rising speed is 4 ℃/10min, and the vacuum degree is kept at 10 Pa; s2, raising the temperature from-30 ℃ to-10 ℃, wherein the temperature raising speed is 4 ℃/10min, and the vacuum degree is kept between 35 Pa; s3, in the stage from-10 ℃ to 0 ℃, the temperature rising speed is 7 ℃/10min, and the vacuum degree is kept at 60 Pa; s4, heating from 0 deg.C to 28 deg.C at a heating rate of 7 deg.C/10 min and a vacuum degree of 10Pa for 120min, pressurizing to normal pressure, and taking out dried extract.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
Example 3
In this embodiment, in the step (1), the addition amount of ethanol is 11 times of the amount of the hawthorn leaf powder, the concentration of ethanol is 95% wt, and the percolation speed is 3.5 mL/min.
Further, in the step (2), ethanol is recovered from the percolate under reduced pressure, and the percolate is concentrated until the relative density of the concentrated solution A is 1.05, so as to obtain the concentrated solution A. The pressure of the reduced pressure concentration is 500 Pa.
Further, in the step (3), the volume ratio of the concentrated solution A to the added water is 1:1.1, and the volume ratio of the diluent to the petroleum ether is 1: 6.5. The temperature for extraction with petroleum ether was 80 ℃.
Further, in the step (4), the volume ratio of the treatment solution to ethyl acetate is 1: 4.2.
Further, in the step (4), ethyl acetate is adopted to perform ultrasonic extraction on the treatment solution, the power of the ultrasonic extraction is 145w, the ultrasonic frequency is 40kHz, the extraction time is 60min, the ultrasonic extraction adopts interval ultrasonic extraction, the interval time is 90s, and the ultrasonic time is 210s each time.
Further, in the step (5), the pressure of the reduced pressure concentration is 500 Pa.
Further, in the step (5), the concentrated solution B is subjected to vacuum freeze-drying, and the vacuum freeze-drying method includes the following steps:
a1 and the concentrated solution B are concentrated to the water content of less than 60 percent, and then pre-frozen to obtain pre-frozen extract A1, wherein the pre-freezing time is-20 ℃, and the pre-freezing time is 75 min;
a2, freezing the pre-frozen extract A1 in vacuum freeze-drying equipment at-35 deg.C under vacuum degree of 100Pa for 50min to obtain extract A2;
a3, cooling to-50 deg.C, vacuum-pumping for sublimation drying, maintaining negative pressure for 60min when the temperature reaches 34 deg.C, pressurizing to normal pressure, and taking out the dried extract.
Further, the step a3 is specifically: reducing the temperature in the vacuum freeze drying equipment to-50 ℃, vacuumizing and carrying out sublimation drying, wherein the temperature rise step is as follows: s1, in the stage process that the temperature is increased from-50 ℃ to-30 ℃, the temperature rising speed is 6 ℃/10min, and the vacuum degree is kept at 30 Pa; s2, raising the temperature from-30 ℃ to-10 ℃, wherein the temperature raising speed is 6 ℃/10min, and the vacuum degree is kept between 55 Pa; s3, in the stage from-10 ℃ to 0 ℃, the temperature rising speed is 9 ℃/10min, and the vacuum degree is kept at 80 Pa; s4, heating from 0 deg.C to 34 deg.C at a heating rate of 9 deg.C/10 min and a vacuum degree of 30Pa for 60min, pressurizing to normal pressure, and taking out dried extract.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
Example 4
In this embodiment, in the step (1), the amount of ethanol added is 9-11 times of the amount of the hawthorn leaf powder, the concentration of ethanol is 95% wt, and the percolation rate is 3.2 mL/min.
Further, in the step (2), ethanol is recovered from the percolate under reduced pressure, and the percolate is concentrated until the relative density of the concentrated solution A is 1.035, so as to obtain the concentrated solution A. In the step (2), the pressure for the concentration under reduced pressure is 350 Pa.
Further, in the step (3), the temperature for extraction with petroleum ether is 75 ℃.
Further, in the step (4), ethyl acetate is adopted to perform ultrasonic extraction on the treatment solution, the power of the ultrasonic extraction is 135w, the ultrasonic frequency is 35kHz, the extraction time is 40min, the ultrasonic extraction adopts interval ultrasonic extraction, the interval time is 70s, and each ultrasonic extraction is 200 s.
Further, in the step (5), the pressure of the reduced pressure concentration is 350 Pa.
Further, in the step (5), the concentrated solution B is subjected to vacuum freeze-drying, and the vacuum freeze-drying method includes the following steps:
a1 and the concentrated solution B are concentrated to the water content of less than 60 percent, and then pre-frozen to obtain pre-frozen extract A1, wherein the pre-freezing time is-22 ℃, and the pre-freezing time is 50 min;
a2, freezing the pre-frozen extract A1 in vacuum freeze-drying equipment at-42 deg.C under vacuum degree of 60Pa for 100min to obtain extract A2;
a3, cooling to-52 deg.C, vacuum-pumping for sublimation drying, maintaining negative pressure for 75min when the temperature reaches 32 deg.C, pressurizing to normal pressure, and taking out the dried extract.
Further, the step a3 is specifically: reducing the temperature in the vacuum freeze drying equipment to-52 ℃, vacuumizing and carrying out sublimation drying, wherein the temperature rise step is as follows: s1, in the stage process that the temperature is increased from-50 ℃ to-30 ℃, the temperature rising speed is 5 ℃/10min, and the vacuum degree is kept at 15 Pa; s2, heating from-30 ℃ to-10 ℃, wherein the heating speed is 5 ℃/10min, and the vacuum degree is kept between 50 Pa; s3, in the stage from-10 ℃ to 0 ℃, the temperature rising speed is 8 ℃/10min, and the vacuum degree is kept at 65 Pa; s4, heating from 0 deg.C to 32 deg.C at a heating rate of 8 deg.C/10 min and a vacuum degree of 25Pa, maintaining the negative pressure for 80min, pressurizing to normal pressure, and taking out the dried extract.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
Comparative example 1
This comparative example differs from example 1 in that: in the step (2), the treatment solution is subjected to oscillation extraction instead of ultrasonic extraction by using ethyl acetate, and the extraction time is 45 min.
Comparative example 2
This comparative example differs from example 1 in that: in the step (5), belt drying is adopted to replace vacuum freeze drying, and the belt drying temperature is 70 ℃.
The contents of the total flavone and the hyperin obtained by measuring the examples 1 to 4 and the comparative examples 1 to 2 according to the measuring method of the 2020 version Chinese pharmacopoeia are as follows:
in the hawthorn leaf extract prepared in the embodiments 1-4 of the invention, the total flavone content is more than 90%, and the hyperin content is more than 0.5%, and the extraction method has the advantages of high yield of active ingredients, simple extraction process, high extraction efficiency, convenient operation and control, low production cost and contribution to industrial production.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (10)
1. A method for extracting hawthorn leaf extract is characterized by comprising the following steps: the method comprises the following steps:
(1) pulverizing folium crataegi into folium crataegi powder, percolating with ethanol as solvent, and collecting percolate;
(2) concentrating the percolate under reduced pressure and recovering ethanol to obtain concentrated solution A;
(3) adding water to dilute the concentrated solution A to obtain a diluted solution; extracting the diluent by adopting petroleum ether, and separating a water layer to obtain a treatment solution;
(4) extracting the treatment solution by using ethyl acetate to obtain an extracting solution;
(5) concentrating the extracting solution under reduced pressure and recovering ethyl acetate to obtain a concentrated solution B; drying to obtain folium crataegi extract.
2. The extraction method of the hawthorn leaf extract as claimed in claim 1, wherein the extraction method comprises the following steps: in the step (1), the addition amount of the ethanol is 9-11 times of the amount of the hawthorn leaf powder, and the concentration of the ethanol is 95% by weight.
3. The environmentally reinforced PC/ABS composite of claim 1, wherein: and (2) decompressing the percolate to recover ethanol, and concentrating until the relative density of the concentrated solution A is 1.03-1.05 to obtain the concentrated solution A.
4. The environmentally reinforced PC/ABS composite of claim 1, wherein: in the step (2), the pressure for the reduced pressure concentration is 300-500 Pa.
5. The extraction method of the hawthorn leaf extract as claimed in claim 1, wherein the extraction method comprises the following steps: in the step (3), the volume ratio of the concentrated solution A to the added water is 1:0.9-1.1, and the volume ratio of the diluent to the petroleum ether is 1: 5.5-6.5.
6. The extraction method of the hawthorn leaf extract as claimed in claim 1, wherein the extraction method comprises the following steps: in the step (3), the temperature for extracting by adopting petroleum ether is 65-80 ℃.
7. The extraction method of the hawthorn leaf extract as claimed in claim 1, wherein the extraction method comprises the following steps: in the step (4), the volume ratio of the treatment solution to the ethyl acetate is 1: 3.8-4.2.
8. The extraction method of the hawthorn leaf extract as claimed in claim 1, wherein the extraction method comprises the following steps: in the step (4), ethyl acetate is adopted to carry out ultrasonic extraction on the treatment solution, the power of the ultrasonic extraction is 125-145w, the ultrasonic frequency is 30-40kHz, the extraction time is 30-60min, the ultrasonic extraction adopts interval ultrasonic extraction, the interval time is 60-90s, and the ultrasonic extraction is carried out for 150-210s each time.
9. The extraction method of the hawthorn leaf extract as claimed in claim 1, wherein the extraction method comprises the following steps: in the step (5), the pressure for the reduced pressure concentration is 300-500 Pa.
10. A hawthorn leaf extract is characterized in that: is prepared by the extraction method of the hawthorn leaf extract of any one of claims 1 to 9.
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| CN102552465A (en) * | 2010-12-29 | 2012-07-11 | 四川科伦药物研究有限公司 | Quality test method for hawthorn leaf medicine, hawthorn leaf extractives or products |
| CN103340948A (en) * | 2013-07-18 | 2013-10-09 | 苏州市天灵中药饮片有限公司 | Preparation method of hawthorn leaf extract |
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| Publication number | Priority date | Publication date | Assignee | Title |
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