CN115040443B - Preparation method of Alsophila spinulosa leaf extract - Google Patents
Preparation method of Alsophila spinulosa leaf extract Download PDFInfo
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- CN115040443B CN115040443B CN202210644253.7A CN202210644253A CN115040443B CN 115040443 B CN115040443 B CN 115040443B CN 202210644253 A CN202210644253 A CN 202210644253A CN 115040443 B CN115040443 B CN 115040443B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9741—Pteridophyta [ferns]
- A61K8/9749—Filicopsida or Pteridopsida
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention relates to a preparation method of Alsophila spinulosa leaf extract, which is characterized by comprising the following steps: A. selecting fresh Alsophila spinulosa leaf, cleaning, drying and pulverizing to obtain Alsophila spinulosa leaf powder; B. mixing glycyrrhizic acid and matrine according to a mass ratio of 1:1 to obtain an ionic preparation; then mixing the mixture with deionized water, vacuumizing, and introducing nitrogen to react for 2-15 hours to obtain an ionic liquid; C. adding Alsophila spinulosa leaf powder into ion-like liquid, gradually heating at 10-35 ℃ in subcritical state with temperature range of 200-300 ℃, and extracting for 1-2 hours respectively at each temperature range; extracting to obtain crude extract; D. concentrating the crude extract under vacuum, and freeze crystallizing to obtain Alsophila spinulosa leaf extract. The invention has the advantages of high active substance content in the obtained Alsophila spinulosa leaf extract, no need of removing ions in the product, and convenient application in cosmetics.
Description
Technical Field
The invention relates to the technical field of extraction and preparation of plant active ingredients, in particular to a preparation method of a leaf extract of Alsophila spinulosa.
Background
With the development of technology and the pursuit of consumers for green and natural, the application of technology means to extract active ingredients for cosmetics from plants is receiving increasing market attention. Cyathea spinulosa is a terrestrial tree fern plant from Cyathea family, is an ancient and old species of Chinese generation, and the stems of Cyathea spinulosa are called as dragon bone wind in Chinese medicine, and has the effects of dispelling wind and removing dampness, promoting blood circulation and removing blood stasis, clearing heat and relieving cough. Alsophila spinulosa leaf extract can activate physiological activity of dermis layer cells, promote synthesis of collagen, promote cell regeneration and repair capability, and promote skin toughness and compactness when applied to cosmetic products.
Alsophila spinulosa leaves are rich in alkaloid, steroid, terpenoid, polyphenol, tannin, flavone, etc., but these active components have different solubility, and the alkaloid and tannin are insoluble in water and the solvent allowed by cosmetics, so that it is difficult to extract them simultaneously.
Matrine is an alkaloid extracted from radix Sophorae Flavescentis, and has been reported to have various pharmacological effects including diuretic, antipathogenic, antioxidant, and liver function improving effects. Matrine can exert an anti-inflammatory effect by inhibiting the expression of cellular inflammatory factors such as Interleukin (IL), tumor necrosis factor-alpha (TNF-alpha) and interleukin receptor. Matrine can also inhibit prostaglandin biosynthesis, which is an inflammatory mediator, and inhibit conversion of arachidonic acid to leukotriene by inhibiting phospholipase and cyclooxygenase, and can also inhibit histamine release from mast cells and directly compete for histamine receptors by stabilizing cell membranes, thereby producing anti-inflammatory effects and having wide anti-inflammatory activity in cosmetics. Glycyrrhizic acid is the most main active ingredient in liquorice, can reduce the reactivity of cells to active factors such as prostaglandin, nonspecific macrophage migration inhibitory factor and the like, and has stronger anti-inflammatory and anti-allergic effects.
At present, the existing extraction method of Alsophila spinulosa generally adopts water extraction or alcohol extraction, and the obtained extract has less active ingredients and low active matter yield. For example, chinese invention patent CN201710048981.0, name: the pure natural pesticide is prepared with 75-86% concentration ethanol and through stirring, soaking, reflux extraction of desmodium and dragon's bone. Chinese invention patent CN201310269528.4, name: a method for extracting oil from wet microalgae mud comprises reacting oil-producing microalgae in subcritical water as extraction medium, ionic liquid as adjuvant, and nitrogen gas under subcritical state; separating after reaction, respectively treating the precipitate and supernatant with lower alkane, evaporating and concentrating the treated alkane phase to obtain microalgae oil and recovering alkane. The ionic liquid is Lewis acidic ionic liquid, lewis alkaline ionic liquid, acidic ionic liquid or alkaline ionic liquid. The method lays the foundation of extracting the ionic liquid in a subcritical state, but the ionic liquid is very wide in variety, and some ionic liquids are poor in extraction effect, so that the ionic liquid cannot be applied in specific formulas and industries due to the fact that common ionic liquids remain, organic solvents such as alkane and the like are required to be used for washing, in addition, different ionic liquids, different temperature and pressure environments can cause different extracted substances, and the method for preparing the Alsophila spinulosa leaf extract which does not need to wash and remove ions and is suitable for the cosmetic industry is developed, so that the method has practical application requirements.
Disclosure of Invention
The invention aims to provide a preparation method of Alsophila spinulosa leaf extract, which can efficiently extract various active substances from Alsophila spinulosa leaves, and the method does not need to remove ions in the product, thereby being convenient for application in cosmetics.
In order to solve the technical problems, the invention adopts the following technical scheme: a preparation method of Alsophila spinulosa leaf extract is characterized by comprising the following steps:
A. selecting fresh Alsophila spinulosa leaves, cleaning, drying in a vacuum drying oven at 40-50 ℃ and under-0.06 Mpa, wherein the drying end point is that the water content is not higher than 5%, the drying time is about 5-8 hours, and then mechanically crushing and sieving with a 60-80 mesh sieve to obtain Alsophila spinulosa leaf powder;
B. mixing glycyrrhizic acid and matrine according to a mass ratio of 1:1 to obtain an ionic preparation; mixing the ionic preparation with deionized water according to a mass ratio of 1-8:100, vacuumizing after uniformly mixing, and then charging nitrogen for reaction for 2-15 hours to obtain an ionic liquid;
C. adding Alsophila spinulosa leaf powder obtained in the step A into the ionic liquid obtained in the step B, gradually heating the ionic liquid in a subcritical state with the temperature range of 200-300 ℃ by taking 10-35 ℃ as a unit, and extracting each temperature range for 1-2 hours respectively; extracting to obtain crude extract;
D. concentrating the crude extract obtained in the step C under vacuum until the water content is lower than 20%, thereby obtaining Alsophila spinulosa leaf extract.
In the step B, the reaction time is 2-3 hours after the nitrogen is filled, and the ionic liquid is obtained after the reaction is completed.
Further, in the step C, the mass ratio of the Alsophila spinulosa leaf powder to the ion-like liquid is 1:5-20.
The Alsophila spinulosa leaf extract prepared by the method is rich in alkaloid, steroid, terpenes, polyphenol, tannin, flavone and other substances, wherein the extraction rate of the alkaloid is 0.7-1.2%, the extraction rate of the steroid is 0.6-1%, the extraction rate of the terpenes is 0.3-0.6%, the extraction rate of the polyphenol is 1.2-2%, the extraction rate of the tannin is 0.4-0.7%, and the extraction rate of the flavone is 1.9-3.8%, so that ions in products can be removed, and the Alsophila spinulosa leaf extract can be conveniently added into cosmetics.
The vacuum drying oven adopted by the invention is a DZF-1 vertical vacuum drying oven, and the manufacturer is Beijing Lin mao science and technology company.
The subcritical extraction equipment adopted by the invention is a CBE-5L subcritical fluid extraction test device, and the manufacturer is Henan province subcritical biotechnology Co.
Under the condition that other experimental conditions are the same, the invention adopts plasma preparations such as glycyrrhizic acid and matrine, salicylic acid and matrine, glycyrrhizic acid and betaine to extract Alsophila spinulosa leaves respectively, the specific experimental conditions are the same as those of example 1, the experimental results are shown in table 1, and the contents of alkaloid (g), steroid compound (g), terpenoid (g), polyphenol (g), tannin (g) and flavonoid (g) in the extracts obtained in each example and comparative example shown in table 1 are converted by HPLC chromatographic experiments. From the data in table 1, compared with an extraction system without adding ionic liquid or with other ionic liquids, the extraction method adopting glycyrrhizic acid and matrine as the ionic preparation can respectively improve the extraction efficiency of alkaloids, polyphenols and tannins by 5-100 times.
TABLE 1 active content of the extracts under different extraction reagents
The invention can fully extract various active substances with different polarities and hydrophilism by selecting proper ion preparation and extracting the active substances such as alkaloid, polyphenol, tannin and the like in the Alsophila spinulosa leaves in a subcritical state with proper temperature. The invention adopts glycyrrhizic acid and matrine as specific ion systems, has smaller molecular steric hindrance, expands the extraction range, particularly extracts alkaloid, polyphenol and tannin in Alsophila spinulosa leaves, and can respectively improve the extraction efficiency of the alkaloid, polyphenol and tannin by 5-100 times compared with the extraction systems without adding ionic liquid or other ionic liquids through HPLC chromatographic experiment contrast and finishing. Matrine and glycyrrhizic acid are common active substances in cosmetics in the market, and can be added into a cosmetic formula without further removing ions in the product.
The invention has the beneficial effects that:
1) Provides a method for efficiently extracting various active substances from Alsophila spinulosa;
2) The raw materials are economical and easy to obtain, and the extraction process is environment-friendly and pollution-free;
3) The invention is suitable for industrial production, has simple and convenient operation and higher efficiency;
4) The combination of matrine and glycyrrhizic acid can provide an ion system to increase the extraction rate, and can be applied to a cosmetic formula together with the Alsophila spinulosa extract, so that the synergistic effect is achieved.
Detailed Description
For the purpose of describing in detail the objects, technical contents and effects achieved by the present invention, the following description will be made with reference to the embodiments. The following examples are merely illustrative of the present invention for the purpose of understanding and are not intended to limit the invention.
Example 1: a preparation method of Alsophila spinulosa leaf extract comprises the following steps:
A. taking fresh Alsophila spinulosa leaves, cleaning, placing in a vacuum drying oven at 50 ℃ under-0.06 mpa, drying for 5 hours until the moisture content is not higher than 5%, mechanically crushing, and sieving with a 60-mesh sieve to obtain 100g Alsophila spinulosa leaf powder;
B. adding 6g of glycyrrhizic acid into 600g of deionized water, stirring until the mixture is uniform, adding 6g of matrine, vacuumizing under-0.06 Mpa, and charging nitrogen gas to react for 2 hours under normal pressure to prepare an ionic liquid;
C. b, screening and extracting Alsophila spinulosa active substances respectively at intervals of 13 ℃ in a subcritical state of the ionic liquid obtained in the step B at 200-300 ℃, wherein the temperature change is 1 hour;
D. concentrating under vacuum until the water content is lower than 20%, to obtain 3.551g of Alsophila spinulosa active substance extract with an active substance extraction efficiency of about 3.55%. Through analytical experiments, the amounts of the respective active substances are shown in the following table:
example 2: a preparation method of Alsophila spinulosa leaf extract comprises the following steps:
A. taking fresh Alsophila spinulosa leaves, cleaning, placing in a vacuum drying oven at 50 ℃ under-0.06 mpa, drying for 5 hours until the moisture content is not higher than 5%, mechanically crushing, and sieving with an 80-mesh sieve to obtain 50g Alsophila spinulosa leaf powder;
B. adding 6g of glycyrrhizic acid into 800g of deionized water, stirring until the mixture is uniform, adding 6g of matrine, vacuumizing under-0.06 Mpa, and charging nitrogen gas to react for 2.5h under normal pressure to prepare an ionic liquid;
C. b, screening and extracting Alsophila spinulosa active substances respectively at intervals of 20 ℃ in a subcritical state of the ionic liquid obtained in the step B at 200-300 ℃, wherein the temperature change is 1 hour;
D. concentrating under vacuum until the water content is lower than 20%, to obtain Alsophila spinulosa active extract 0.853g with active extraction efficiency of about 1.71%. Through analytical experiments, the amounts of the respective active substances are shown in the following table:
example 3: a preparation method of Alsophila spinulosa leaf extract comprises the following steps;
A. taking fresh Alsophila spinulosa leaves, cleaning, placing in a vacuum drying oven at 50 ℃ under-0.06 mpa, drying for 8 hours until the moisture content is not higher than 5%, mechanically crushing, and sieving with an 80-mesh sieve to obtain 1500g Alsophila spinulosa leaf powder;
B. adding 60g of glycyrrhizic acid into 7200g of deionized water, stirring until the mixture is uniform, adding 60g of matrine, vacuumizing under-0.06 Mpa, and charging nitrogen gas to react for 5 hours under normal pressure to prepare an ionic liquid;
C. b, screening and extracting Alsophila spinulosa active substances respectively at intervals of 15 ℃ in a subcritical state of the ionic liquid obtained in the step B at 200-300 ℃, wherein the temperature change is 1.5 hours;
D. concentrating under vacuum until the water content is lower than 20%, to obtain 49.56g of Alsophila spinulosa active substance extract with an active substance extraction efficiency of about 3.30%. Through analytical experiments, the amounts of the respective active substances are shown in the following table:
example 4: a preparation method of Alsophila spinulosa leaf extract comprises the following steps:
A. taking fresh Alsophila spinulosa leaves, cleaning, placing in a vacuum drying oven at 50 ℃ under-0.06 mpa, drying for 6 hours until the moisture content is not higher than 5%, mechanically crushing, and sieving with an 80-mesh sieve to obtain 600g Alsophila spinulosa leaf powder;
B. adding 50g of glycyrrhizic acid into 800g of deionized water, stirring until the mixture is uniform, adding 50g of matrine, vacuumizing under-0.06 Mpa, and charging nitrogen gas to react for 3 hours under normal pressure to prepare an ionic liquid;
C. b, screening and extracting Alsophila spinulosa active substances respectively at intervals of 35 ℃ in a subcritical state of the ionic liquid obtained in the step B at 200-300 ℃, wherein the temperature change is 1 hour;
D. concentrating under vacuum until the water content is lower than 20%, to obtain 10.736g of Alsophila spinulosa active substance extract with active substance extraction efficiency of about 1.79%. Through analytical experiments, the amounts of the respective active substances are shown in the following table:
example 5: a preparation method of Alsophila spinulosa leaf extract comprises the following steps:
A. taking fresh Alsophila spinulosa leaves, cleaning, placing in a vacuum drying oven at 50 ℃ under-0.06 mpa, drying for 5.5h until the moisture content is not higher than 5%, mechanically crushing, and sieving with a 80-mesh sieve to obtain 300g Alsophila spinulosa leaf powder;
B. adding 80g of glycyrrhizic acid into 3200g of deionized water, stirring until the mixture is uniform, adding 80g of matrine, vacuumizing under-0.06 Mpa, and charging nitrogen gas to react for 14h at normal pressure to prepare the ionic liquid;
C. b, respectively screening and extracting Alsophila spinulosa active substances at intervals of 20 ℃ in a subcritical state of the ionic liquid obtained in the step B at 200-300 ℃, wherein the temperature change is in units of 2 hours;
D. concentrating under vacuum until the water content is lower than 20%, to obtain 10.045g of Alsophila spinulosa active substance extract with an active substance extraction efficiency of about 3.35%. Through analytical experiments, the amounts of the respective active substances are shown in the following table:
example 6: a preparation method of Alsophila spinulosa leaf extract comprises the following steps:
A. taking fresh Alsophila spinulosa leaves, cleaning, placing in a vacuum drying oven at-0.06 Mpa and 40 ℃ for drying for 5 hours, wherein the drying end point is that the water content is not higher than 5%, mechanically crushing, and sieving with a 60-mesh sieve to obtain 350g Alsophila spinulosa leaf powder;
B. 200g of glycyrrhizic acid is added into 6600g of deionized water, 200g of matrine is added after stirring evenly, vacuum pumping is carried out under-0.06 Mpa, nitrogen is filled into the deionized water for reaction for 9h under normal pressure, and ion-like liquid is prepared;
C. b, screening and extracting Alsophila spinulosa active substances respectively at intervals of 10 ℃ in a subcritical state of the ionic liquid obtained in the step B at 200-300 ℃, wherein the temperature change is 1 hour;
D. concentrating under vacuum until the water content is lower than 20%, to obtain 10.817g of Alsophila spinulosa active substance extract with an active substance extraction efficiency of about 3.09%. Through analytical experiments, the amounts of the respective active substances are shown in the following table:
Claims (2)
1. a preparation method of Alsophila spinulosa leaf extract is characterized by comprising the following steps:
A. selecting fresh Alsophila spinulosa leaves, cleaning, drying in a vacuum drying oven at 40-50 ℃ and under-0.06 Mpa, wherein the drying end point is that the moisture content is not higher than 5%, mechanically crushing, and sieving with a 60-80 mesh sieve to obtain Alsophila spinulosa leaf powder;
B. mixing glycyrrhizic acid and matrine according to a mass ratio of 1:1 to obtain an ionic preparation; mixing the ionic preparation with deionized water according to a mass ratio of 1-8:100, vacuumizing after uniformly mixing, and then charging nitrogen for reaction for 2-15 hours to obtain an ionic liquid;
C. adding Alsophila spinulosa leaf powder obtained in the step A into the ionic liquid obtained in the step B, gradually heating the ionic liquid in a subcritical state with the temperature range of 200-300 ℃ by taking 10-35 ℃ as a unit, and extracting each temperature range for 1-2 hours respectively; extracting to obtain crude extract; the mass ratio of the Alsophila spinulosa leaf powder to the ion-like liquid is 1:5-20;
D. concentrating the crude extract obtained in the step C under vacuum until the water content is lower than 20%, thereby obtaining Alsophila spinulosa leaf extract.
2. The method for preparing the extract of Alsophila spinulosa leaves according to claim 1, characterized in that: in the step B, the reaction time is 2-3 hours after nitrogen is filled, and the ionic liquid is obtained after the reaction is completed.
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