CN116650547A - Method for extracting flavone from snow lotus herb - Google Patents
Method for extracting flavone from snow lotus herb Download PDFInfo
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- CN116650547A CN116650547A CN202310718816.7A CN202310718816A CN116650547A CN 116650547 A CN116650547 A CN 116650547A CN 202310718816 A CN202310718816 A CN 202310718816A CN 116650547 A CN116650547 A CN 116650547A
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- extraction
- flavone
- snow lotus
- extracting
- herba saussureae
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- 229930003944 flavone Natural products 0.000 title claims abstract description 43
- 235000011949 flavones Nutrition 0.000 title claims abstract description 43
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 title claims abstract description 39
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 39
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 26
- 240000002853 Nelumbo nucifera Species 0.000 title claims description 22
- 235000006508 Nelumbo nucifera Nutrition 0.000 title claims description 22
- 235000006510 Nelumbo pentapetala Nutrition 0.000 title claims description 22
- 238000000605 extraction Methods 0.000 claims abstract description 61
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 48
- 239000000047 product Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000284 extract Substances 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000000746 purification Methods 0.000 abstract description 4
- 238000004904 shortening Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000002904 solvent Substances 0.000 description 8
- 239000011344 liquid material Substances 0.000 description 6
- 239000004480 active ingredient Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 150000002213 flavones Chemical class 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- 229930003935 flavonoid Natural products 0.000 description 3
- 150000002215 flavonoids Chemical class 0.000 description 3
- 235000017173 flavonoids Nutrition 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 241000133134 Saussurea Species 0.000 description 2
- 241001145025 Saussurea involucrata Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 210000003734 kidney Anatomy 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- 241000208838 Asteraceae Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000032843 Hemorrhage Diseases 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 206010053476 Traumatic haemorrhage Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000005906 menstruation Effects 0.000 description 1
- 239000000401 methanolic extract Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 210000002435 tendon Anatomy 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
- A61K36/285—Aucklandia
-
- 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
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Pyrane Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting flavone from herba Saussureae Involueratae, which is used for realizing rapid and efficient extraction of flavone products, simplifying the extraction process, shortening the extraction and purification time, reducing the production cost, and the extracted flavone has high yield, good quality and high purity.
Description
Technical Field
The invention belongs to the technical field of organic matter extraction, and particularly relates to a method for extracting flavone from snow lotus herb.
Background
Herba Saussureae Involueratae is herb of saussurea of Compositae for many years. The snow lotus stem has no hair, leaves are elliptical or oval, two sides have no hair, the uppermost part is She Baoshe-shaped, the wide oval shape is formed, the head inflorescences are densely integrated into a spherical total inflorescence at the top of the stem, the outer layer is oblong, the fruits are oblong, and the flower and fruit period is 7-9 months. The herba Saussureae Involueratae herb can be used as common medicine for Uygur nationality, etc., has effects of warming, slightly bitter, nourishing liver and kidney channel, dispelling pathogenic wind and dampness, strengthening tendons and bones, invigorating kidney yang, regulating menstruation and stopping bleeding; can be applied externally for traumatic hemorrhage; it is contraindicated for pregnant women.
In the prior art, the method for extracting the flavone mainly comprises a water extraction method, a biological enzyme degradation technology and an ultrasonic extraction technology. The water extraction method is gradually eliminated, the biological enzyme degradation technology has larger limitation, mainly the temperature is not well controlled, if the temperature is too high, the components are easy to degrade, the extraction efficiency is low; if the temperature is too low, the components are not easy to separate, the active ingredients cannot be fully dissolved, and the cost is high.
The extraction method adopted at present mainly comprises an organic solvent extraction method and a supercritical CO2 extraction method. The organic solvent extraction method mainly uses petroleum ether with boiling point of 60-70 ℃ as solvent to repeatedly extract flavone. The method has the defects that firstly, the purity of the product is not high due to the problem of solvent residue; secondly, the volatilization of the solvent in the heating process increases the cost of the product. Supercritical CO 2 The extraction method is currently the more advanced extraction method, which uses supercritical CO 2 Novel technology for extracting plant active ingredients by fluid instead of organic solvent, CO 2 The fluid is nontoxic, nonflammable and explosive, has no damage to active ingredients, no organic solvent residue and high product purity, thus supercritical CO 2 The fluid is suitable for extracting high heat-sensitive substances and separating volatile components. The flavone oil produced by the method has the following defects although the quality is better: firstly, the method has limited daily treatment capacity of the snow lotus flower in the snow lotus flower picking season. The method has the temperature of 35-40 ℃, the one-time extraction time is about 5 hours, and the maximum daily treatment amount is not more than 3 tons, so the method is not suitable for mass production in the rush harvesting season of the snow lotus. Secondly, when the method is used for extracting flavone, the saussurea involucrata is crushed or pressed into tablets, so that the acid value of the product is increased. Thirdly, the production conditions and the corresponding labor protection measures are strict (extraction vessels belong to three types of pressure vessels), expensive and special equipment is required, and therefore, the method is limited in application.
The existing flavone extraction and processing method mainly has the following defects:
1. the acidity is higher during processing, so that harmful substances such as peroxidation substances, potassium acid and the like are increased, the preservation time is shorter after flavone extraction, mildew is easy to generate, and the health is influenced after eating;
2. the effective components of the snow lotus flower are seriously lost during processing, the effective components cannot be fully dissolved, only part of the effective components enter a solvent, so that waste and high product cost are caused;
most of the existing processing methods need to grind snow lotus into powder, a large amount of labor is needed, the production efficiency is low, the labor intensity is high, the loss of active ingredients in the extraction process is serious, and the extraction rate is low.
4. Supercritical extraction equipment is expensive and cannot be widely popularized and used.
Therefore, there is a need to develop a new flavone extraction method to better solve the above problems.
The invention aims to solve the technical problems and provide a method for extracting flavone from saussurea involucrate, which is used for realizing rapid and efficient extraction of flavone products, simplifying the extraction process, shortening the extraction and purification time, reducing the production cost, and has the advantages of high yield, good quality and high purity of the extracted flavone.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for extracting flavone from saussurea involucrata, which is used for realizing rapid and efficient extraction of flavone products, simplifying the extraction process, shortening the extraction and purification time, reducing the production cost, and has the advantages of high yield, good quality and high purity of the extracted flavone.
In order to achieve the above purpose, the invention discloses a method for extracting flavone from herba Saussureae Involueratae, which comprises the following steps:
(1) Weighing 100-500g of snow lotus herb, and crushing;
(2) Adding 0.8-1.5g herba Saussureae Involueratae into 20-50mL methanol solution with volume fraction of 60-100%, shaking in ultrasonic vibrator for 30-90min, and vacuum filtering; repeatedly extracting for 2-6 times, mixing filtrates, distilling, concentrating, and fixing volume with 70% ethanol solution in 20-40m L volumetric flask at 30-80deg.C to obtain extractive solution;
(3) Filtering the extract obtained in the step (2) to remove residues to obtain a flavone product;
preferably, the method specifically comprises the following steps:
(1) The sample is herba Saussureae Involueratae produced in Qinghai region, purchased from local market, and weighed 200g and crushed;
(2) Adding 1.00g of herba Saussureae Involueratae into 100% methanol solution 60m L, shaking in an ultrasonic vibrator for 60min, vacuum filtering, extracting repeatedly for 3 times, mixing filtrates, concentrating by distillation, and fixing volume in 25m L volumetric flask with 70% ethanol solution at 60deg.C to obtain extractive solution;
(3) Filtering the extract to remove residue to obtain flavone product.
The beneficial effects are that:
1) The invention can extract flavone products rapidly and efficiently, simplify the extraction process and shorten the extraction and purification time.
2) The flavone prepared by the invention has high yield, good quality and high purity.
Detailed Description
The following are only preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
EXAMPLE 1 extraction of flavones
(1) The sample is herba Saussureae Involueratae produced in Qinghai region, purchased from local market, and weighed 200g and crushed;
(2) Adding 1.00g of herba Saussureae Involueratae into 100% methanol solution 60m L, shaking in an ultrasonic vibrator for 60min, vacuum filtering, extracting repeatedly for 3 times, mixing filtrates, concentrating by distillation, and fixing volume in 25m L volumetric flask with 70% ethanol solution at 60deg.C to obtain extractive solution;
(3) Filtering the extract to remove residue to obtain flavone product.
Example 2 Effect of methanol mass fraction on the extraction of flavonoids from snow lotus
Under the same extraction conditions (extraction time is 60min, extraction temperature is 60 ℃, liquid-to-material ratio is 100:1), the influence on the comprehensive score of the flavone component in the herba saussureae involucratae is detected when the mass fraction of the methanol is 75%, 80%, 85%, 90%, 95% and 100%, and according to the technical scheme, the comprehensive extraction rate of the flavone is reduced and then increased along with the increase of the mass fraction of the methanol, but when the mass fraction of the methanol reaches 85%, the change of the mass fraction of the methanol has little influence on the extraction rate of the flavone in the herba saussureae involucratae. Because the low-concentration methanol extract is not easy to filter in the experimental process, 100% methanol is comprehensively considered as an extraction solvent.
Example 3 Effect of extraction time on the extraction Effect of flavones in snow lotus flower
Under the same extraction conditions (the mass fraction of methanol is 100%, the extraction temperature is 60 ℃ and the liquid-material ratio is 100:1), when the extraction time is 30, 40, 50, 60, 70 and 80min, the influence on the comprehensive score of the flavone component in the herba saussureae involucratae is detected, and according to the technical scheme, the comprehensive extraction rate of the flavone is reduced firstly and then increased along with the time extension within 30-60 min, and is reduced along with the time extension after 60min, so the extraction time is 60min.
Example 4 Effect of liquid-to-Material ratio on the extraction Effect of flavones in snow lotus flower
Under the same extraction conditions (the mass fraction of methanol is 100%, the extraction temperature is 60 ℃ and the extraction time is 60 min), the influence on the comprehensive score of the flavone component in the snow lotus herb is detected when the liquid-material ratio is 70:1, 80:1, 90:1, 100:1, 110:1 and 120:1 (mL/g), the technical scheme proves that when the liquid-material ratio is increased, the amount of the solvent which can dissolve the flavone is increased, but when the solvent exceeds a certain volume, the solvent can produce a dilution effect on the solution, and the cost is considered to select the liquid-material ratio to be 70:1 (mL/g).
Example 5 Effect of extraction temperature on the extraction Effect of flavones in snow lotus flower
Under the same extraction conditions (the mass fraction of methanol is 100%, the extraction time is 60min, the liquid-material ratio is 100:1), the influence on the comprehensive score of the flavone component in the snow lotus herb is detected when the extraction temperature is 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃ and 80 ℃, and according to the technical scheme, the molecular movement can be promoted by increasing the extraction temperature, the dissolution of the effective component is accelerated, the dissolution rate of the effective component is not increased after the extraction temperature reaches a certain value, the influence on the dissolution of the component by increasing the temperature is small after the extraction temperature reaches 70 ℃, and the extraction temperature is selected to be 60 ℃ by comprehensively considering the extraction temperature.
The invention carries out single factor detection on the extraction time, the extraction temperature, the liquid-material ratio and the mass fraction of methanol, and firstly uses the analytic hierarchy process to determine the weight of extracting the flavone from the snow lotus herb to reach the optimal technical evaluation index, so that the evaluation index is more scientific and reasonable, and finally adopts uniform design to determine the optimal technological conditions of ultrasonically extracting the flavone component in the snow lotus herb as follows: the extraction temperature is 60 ℃, the extraction time is 70min, the liquid-to-material ratio is 60:1 (mL/g), and the mass fraction of methanol is 100%. The verification test result and the prediction comprehensive score have little difference, and the method for optimizing the extraction process of the flavonoid component in the snow lotus herb by using the uniform design method is proved to be feasible, and the technical scheme of the invention can provide guiding significance for the improvement of the extraction method and process of the flavonoid in the future.
Claims (2)
1. The method for extracting the flavone from the snow lotus herb is characterized by comprising the following steps of:
(1) Weighing 100-500g of snow lotus herb, and crushing;
(2) Adding 0.8-1.5g herba Saussureae Involueratae into 20-50mL methanol solution with volume fraction of 60-100%, shaking in ultrasonic vibrator for 30-90min, and vacuum filtering; repeating extraction for 2-6 times, mixing filtrates, distilling, concentrating, and fixing volume with 70% ethanol solution in 20-40mL volumetric flask at 30-80deg.C to obtain extractive solution;
(3) Filtering the extract obtained in the step (2) to remove residues, and obtaining a flavone product.
2. The method for extracting the flavone from the snow lotus herb is characterized by comprising the following steps of:
(1) Selecting herba Saussureae Involueratae produced in Qinghai region, weighing 200g, and pulverizing;
(2) Adding 1.00g of herba Saussureae Involueratae into 60mL of 100% methanol solution, shaking in an ultrasonic vibrator for 60min, vacuum filtering, extracting repeatedly for 3 times, mixing filtrates, concentrating by distillation, and fixing volume in 25mL volumetric flask with 70% ethanol solution at 60deg.C to obtain extractive solution;
(3) Filtering the extractive solution to remove residue to obtain flavone product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310718816.7A CN116650547A (en) | 2023-06-16 | 2023-06-16 | Method for extracting flavone from snow lotus herb |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310718816.7A CN116650547A (en) | 2023-06-16 | 2023-06-16 | Method for extracting flavone from snow lotus herb |
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| Publication Number | Publication Date |
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| CN116650547A true CN116650547A (en) | 2023-08-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310718816.7A Pending CN116650547A (en) | 2023-06-16 | 2023-06-16 | Method for extracting flavone from snow lotus herb |
Country Status (1)
| Country | Link |
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| CN (1) | CN116650547A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686357A (en) * | 2005-03-25 | 2005-10-26 | 张海峰 | Saussurea involucrate powder injection and its preparation method |
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- 2023-06-16 CN CN202310718816.7A patent/CN116650547A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686357A (en) * | 2005-03-25 | 2005-10-26 | 张海峰 | Saussurea involucrate powder injection and its preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 史俊友;景年华;汪帆;赵红艳;杨晓丽;: "3种雪莲总黄酮含量及其抗氧化活性比较", 中成药, no. 08, 20 August 2013 (2013-08-20), pages 1813 - 1815 * |
| 韩鸿萍;王发春;: "水母雪莲花中总黄酮的提取工艺及含量测定研究", 青海师范大学学报(自然科学版), no. 03, 15 September 2010 (2010-09-15), pages 68 - 69 * |
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