阅读说明：本技术 一种从沉香叶中提取防晒成分的方法及防晒组合物 (Method for extracting sunscreen component from agilawood leaves and sunscreen composition ) 是由 陈绍昌 于 2021-07-23 设计创作，主要内容包括：本发明公开了一种从沉香叶中提取防晒成分的方法及防晒组合物。提取方法包括以下步骤：将沉香叶清洗,干燥,粉碎并过筛,获得沉香叶粉末；按料液比为1g：(30～60)ml向沉香叶粉末中加入体积比为30～60％的碱性乙醇溶液,在超声条件下进行提取,过滤；将得到的滤液减压浓缩至无醇味,即得沉香叶提取物。本发明采用碱性乙醇作为提取溶剂,并以甘氨酸-氯化钠-NaOH溶液为碱性缓冲溶液,原料来源稳定成本更低,提取更充分,有利于防晒成分的提取。本发明提供的防晒剂来源天然,对皮肤刺激性小、作用温和、安全性高；不仅具有良好的防晒性能,而且具有良好的美白、抗氧化等性能。(The invention discloses a method for extracting a sun-screening component from agilawood leaves and a sun-screening composition. The extraction method comprises the following steps: cleaning the agilawood leaves, drying, crushing and sieving to obtain agilawood leaf powder; according to the material-liquid ratio of 1 g: (30-60) ml of alkaline ethanol solution with the volume ratio of 30-60% is added into the agilawood leaf powder, extraction is carried out under the ultrasonic condition, and filtering is carried out; concentrating the filtrate under reduced pressure until no alcohol smell exists to obtain folium Aquilariae Resinatum extract. The invention adopts alkaline ethanol as an extraction solvent and glycine-sodium chloride-NaOH solution as an alkaline buffer solution, has stable raw material source, lower cost and more sufficient extraction, and is beneficial to the extraction of sunscreen components. The sunscreen agent provided by the invention is natural in source, small in skin irritation, mild in action and high in safety; the sun-screening agent has good sun-screening performance, and has good whitening, oxidation resistance and other performances.)

1. A method for extracting a sunscreen component from agilawood leaves is characterized by comprising the following steps:

(1) picking and collecting agilawood leaves, cleaning, drying, crushing and sieving to obtain agilawood leaf powder;

(2) according to the material-liquid ratio of 1 g: (30-60) ml of alkaline ethanol solution with the volume ratio of 30-60% is added into the agilawood leaf powder, extraction is carried out under the ultrasonic condition, and then filtration is carried out; concentrating the filtrate under reduced pressure until no alcohol smell exists to obtain folium Aquilariae Resinatum extract.

2. The method for extracting sunscreen ingredients from aquilaria sinensis leaves as claimed in claim 1, wherein the alkaline ethanol solution in the step (2) is prepared by mixing absolute ethanol and alkaline buffer solution; the alkaline buffer solution is glycine-sodium chloride-NaOH solution.

3. The method for extracting sunscreen ingredients from agilawood leaves according to claim 1, wherein the pH value of the alkaline ethanol solution in the step (2) is 11-12.

4. The method for extracting sunscreen ingredients from agilawood leaves according to claim 1, wherein the material-liquid ratio in step (2) is 1 g: 45 mL; the volume ratio of the alkaline ethanol solution is 40%.

5. The method for extracting the sun-screening components from the aquilaria sinensis leaves as claimed in claim 1, wherein the ultrasonic wave in the step (2) has the power of 48-500W and the frequency of 25-80 KHz; the extraction temperature is 30-80 ℃, and the extraction time is 30-90 min/time.

6. The method for extracting sun-screening ingredients from aquilaria sinensis leaves as claimed in claim 1, wherein in the step (2), the power of the ultrasonic wave is 60W-180W, and the frequency is 25-80 KHz; the extraction time is 30-70 min/time, and the extraction temperature is 30-70 ℃.

7. The method for extracting sun-screening ingredients from aquilaria sinensis leaves as claimed in claim 1, wherein in the step (2), the extraction time is 50 min/time, and the extraction temperature is 70 ℃.

8. An extract from aquilaria sinensis leaves, which is obtained by the method according to any one of claims 1 to 7.

9. A sunscreen composition comprising from 0.1 wt.% to 25 wt.% of the eaglewood leaf extract of claim 8.

10. A sunscreen composition according to claim 9, characterized in that said sunscreen composition comprises from 1 wt.% to 10 wt.% of said eaglewood leaf extract according to claim 8.

Technical Field

The invention belongs to the technical field of natural product separation, and particularly relates to a method for extracting a sun-screening component from agilawood leaves and a sun-screening composition.

Background

Atmospheric pollution causes ozone layer to be destroyed, the intensity of ultraviolet radiation reaching the ground is continuously increased, and people face more serious threat of ultraviolet injury. The damage mainly comes from long-wave ultraviolet rays (UVA, 320-400 nm) and medium-wave ultraviolet rays (UVB, 290-320 nm). UVB penetrates the epidermal and stratum corneum layers of the skin and is the major source of skin burns, indirect pigmentation, and skin cancer. UVA can reach the dermis layer of the skin, and is the main cause of skin aging.

The natural sunscreen agent is an active ingredient extracted from natural animals and plants and capable of effectively absorbing ultraviolet rays and scavenging free radicals. Unlike chemical synthesized sunscreens such as benzophenone derivatives and cinnamate, natural sunscreens have single functions and even potential risks. The natural sun-screening agent has the advantages of good ultraviolet absorption capacity, low sensitization rate, high safety, small skin irritation, mild effect, most of effects of scavenging oxygen free radicals, resisting bacteria, resisting inflammation and the like, and wide application prospect.

Lignum Aquilariae Resinatum is also called Aquilaria sinensis (Lour.) Gilg, and is a plant of Aquilaria of Thymelaeaceae, and its resin-containing wood is a famous Chinese medicinal material, and has effects of activating qi-flowing, relieving pain, warming middle warmer, relieving vomit, promoting inspiration, and relieving asthma, and can be used for treating chest and abdomen distention pain, stomach cold emesis, singultus, and deficiency of the kidney. However, the agilawood is a tall tree, grows slowly, has long hardening time and has long period of generating economic benefit. And the agilawood only contains wood containing resin for medical use, and other parts such as leaves, branches and wood without resin are treated as waste. The agilawood leaves serving as non-medicinal parts of the agilawood can be picked twice a year, the yield is high, but the agilawood leaves are often used as waste to be treated, so that the resource waste is caused. Eaglewood leaf is regarded by researchers as having a plurality of pharmacological actions such as oxidation resistance, blood sugar and blood fat reduction, inflammation resistance, asthma relief and the like. Modern researches show that the chemical components of the agilawood leaves mainly comprise polyphenols, flavones and glycosides thereof, benzophenone derivatives, tanshinone and the like. Mangiferin is a polyphenol substance with the highest content in the aquilaria sinensis, is a natural antioxidant for removing free radicals, is also a natural radiation protective agent, 4 phenolic hydroxyl groups in the molecular structure of the mangiferin have electrophilic capacity, and a benzene ring is a good energy trap, so that free radicals initiated by irradiation of biomolecules can be transferred to a certain extent, and the biomolecules are protected. In addition, flavone and its glycosides, benzophenone derivatives, etc. also have effects of absorbing ultraviolet, scavenging free radicals, resisting oxidation, and resisting virus.

CN200710019969.3 discloses a agilawood leaf extract and medical and health care applications thereof; CN201410803301.8 discloses the use of an extract of agilawood leaves as an active ingredient for whitening. However, the use of the extract of Aquilaria sinensis as a sunscreen agent has not been reported.

Disclosure of Invention

The currently widely used neutral ethanol solution extraction method cannot fully extract the effective components of the agilawood leaves. In order to overcome the defects and shortcomings in the prior art, the invention provides a method for keeping the pH value basically stable and fully extracting the functional components, so that the pH value of the extracting solution is not greatly changed in the whole extraction process, and the sun-screening components in the aquilaria sinensis can be fully extracted.

It is another object of the present invention to provide a sunscreen composition.

The purpose of the invention is realized by the following technical scheme:

a method for extracting sunscreen components from folium Aquilariae Resinatum comprises the following steps:

(1) picking and collecting agilawood leaves, cleaning, drying to remove water, crushing and sieving to obtain agilawood leaf powder;

(2) according to the material-liquid ratio of 1 g: (30-60) ml of alkaline ethanol solution with the volume ratio of 30-60% is added into the agilawood leaf powder, extraction is carried out under the ultrasonic condition, and then filtration is carried out; concentrating the filtrate under reduced pressure until no alcohol smell exists to obtain folium Aquilariae Resinatum extract. The ethanol can be recycled.

The drying in the step (1) is to remove moisture contained on the surface of the agilawood leaves and the agilawood leaves by airing or drying, and comprises a natural airing or low-temperature drying mode.

Further, the sieving in the step (1) refers to sieving through a 100-mesh sieve.

Further, the volume ratio of the alkaline ethanol solution in the step (2) is 40%.

Further, the alkaline ethanol solution in the step (2) is prepared by absolute ethanol and an alkaline buffer solution.

The alkaline buffer solution is preferably glycine-sodium chloride-NaOH solution.

Further, the pH value of the alkaline ethanol solution in the step (2) is 11-12, and is preferably 11.6.

Further, the feed-liquid ratio in the step (2) is preferably 1 g: 45 mL.

Further, the power of the ultrasound in the step (2) is 48-500W, preferably 60-180W, and more preferably 80W; the frequency of the ultrasonic wave is 25-80 KHz.

Further, the extraction temperature in the step (2) is 30-80 ℃, preferably 30-70 ℃, and more preferably 70 ℃; the extraction time is 30-90 min/time, preferably 30-70 min/time, and more preferably 50 min/time.

Further, in the step (2), the extraction is performed for 1-3 times under the ultrasonic condition.

Further, the temperature of the concentration under reduced pressure in the step (2) is 60 ℃.

According to the eaglewood leaf extract obtained by the method, the sunscreen substances contained in the eaglewood leaf extract can be divided into polyphenols, flavones and glycosides thereof, benzophenone derivatives, tanshinone and the like according to the structure, and can be applied to sunscreen cosmetics.

The present invention also provides a sunscreen composition comprising the extract of agilawood leaves obtained by the method of the present invention as a sunscreen ingredient in an amount of from 0.1 wt.% to 25 wt.%, preferably in an amount of from 1 wt.% to 10 wt.%.

Preferably, general ingredients suitable for sunscreen cosmetics, such as a humectant, an emollient, water, an emulsifier and other matrix ingredients, are also added to the sunscreen composition.

Preferably, the formulation of the sunscreen composition is not particularly limited, and may be a solution, an emulsion, a cream, a spray, and the like.

Compared with the prior art, the invention has the following advantages and beneficial effects:

according to the invention, the agilawood leaves are taken as the raw materials for extracting the sunscreen agent, so that the limitation of the raw materials is broken through, the economic value of agilawood planting production is improved, and the waste is changed into valuable; according to the characteristics of the raw materials, ethanol is used as an extraction solvent, and a glycine-sodium chloride-NaOH solution is used as an alkaline buffer solution, so that the raw materials are stable in source, low in cost and sufficient in extraction, and extraction of sunscreen components is facilitated.

The sunscreen agent provided by the invention is natural in source, small in skin irritation, mild in action and high in safety; the sunscreen agent has good sunscreen performance, good whitening, oxidation resistance and other performances, and meets the requirements of people on safety, environmental protection and multiple effects of the sunscreen agent.

Detailed Description

The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The raw materials related to the invention can be directly purchased from the market. For process parameters not specifically noted, reference may be made to conventional techniques.

In order to study the influence of the process parameters of the method for extracting the sunscreen components from the aquilaria sinensis leaves on the sunscreen effect of the extract, the following experiments were carried out:

in the following experiments, the 40% (volume) alkaline ethanol solution is prepared by absolute ethyl alcohol and an alkaline buffer solution, the pH value is 11-12, and the percentage refers to volume percentage; the alkaline buffer solution is glycine-sodium chloride-NaOH solution.

1) Effect of extraction solvent on sunscreen Activity of extract

Picking and collecting agilawood leaves, cleaning, airing or drying to remove water in the agilawood leaves, crushing, and sieving with a 100-mesh sieve; accurately weighing 4 parts of 1.0g of agilawood leaf powder into a 100mL round-bottom flask, respectively adding 45mL of distilled water, 40% (volume) ethanol water solution, 40% (volume) acidic ethanol solution and 40% (volume) alkaline ethanol solution, performing ultrasonic extraction for 50min under the ultrasonic conditions of 50 ℃ temperature, 120W of power and 25KHz of frequency, performing suction filtration, collecting filtrate, and using a corresponding extraction solvent to fix the volume to 100 mL. Measuring the absorbance of the extract at a wavelength of 200-400 nm, calculating the average absorbance values of UVC (200-290 nm), UVB (290-320 nm) and UVA (320-400 nm), and evaluating the ultraviolet absorption capacity, namely the sunscreen capacity.

TABLE 1 selection of extraction solvents

As can be seen from Table 1, in the method of the present invention, eaglewood leaves are used as raw materials, and when an alkaline ethanol solution is used as an extraction agent, the absorbance of the extraction solution is significantly higher in both UVA region and UVB region than in a neutral ethanol solution and an acidic ethanol solution, which indicates that the dissolution of effective components such as polyphenols and organic acids in eaglewood leaves is not favored in acidic and neutral media. If the extractant is too basic or too weak, the absorbance in the UVA region is reduced to some extent. When a basic ethanol solution is used as an extractant, the basic ethanol solution becomes gradually less basic during the extraction process.

2) Influence of volume ratio of ethanol on sunscreen activity of folium Aquilariae Resinatum extractive solution

Accurately weighing 1.00g of dried eaglewood leaf powder into 5 100mL round-bottom flasks, adding 45mL of alkaline ethanol solutions with different volume ratios, performing ultrasonic reflux for 50min under the ultrasonic conditions of power of 120W, frequency of 25KHz and temperature of 70 ℃, performing suction filtration, collecting filtrate, performing constant volume by using the alkaline ethanol solutions with corresponding volume ratios, measuring the absorbance of the extracting solution in the wavelength range of 200-400 nm, calculating the average absorbance values of UVC (200-290 nm), UVB (290-320 nm) and UVA (320-400 nm), and comparing the ultraviolet absorption capacities, wherein the results are shown in Table 2.

TABLE 2 influence of the volume ratio of the alkaline ethanol solution on the sunscreen activity of the extract of Aquilaria sinensis

As can be seen from the results in table 2, the average absorbance of the extract of eaglewood leaves obtained by extracting with different volume ratios of the alkaline ethanol solution starts to increase with the increase of the concentration, but when the volume ratio of the alkaline ethanol solution exceeds 40%, the absorbance is obviously reduced. When the volume ratio of the alkaline ethanol solution exceeds 40%, the average absorbance of the agilawood leaf extracting solution reaches the maximum, which shows that when the volume ratio of the alkaline ethanol solution is 40%, the sunscreen active matters in the agilawood leaves can be sufficiently extracted, and if the volume ratio of the alkaline ethanol solution is increased, the average absorbance of the extracting solution is not increased, but the ethanol is wasted, so that the optimum volume ratio of the alkaline ethanol solution is 40%.

3) Influence of feed liquid ratio on sunscreen activity of agilawood leaf extracting solution

Accurately weighing 0.20g, 0.40g, 0.60g, 0.80g, 1.00g and 1.20g of dried eaglewood leaf powder into 6 100mL round-bottom flasks, respectively adding 45mL 40% (volume) of alkaline ethanol solution, refluxing for 50min under the ultrasonic conditions of 80W power, 80KHz frequency and 70 ℃, filtering, collecting filtrate, fixing the volume by using 40% (volume) of alkaline ethanol solution, measuring the absorbance of the extracting solution in the wavelength range of 200-400 nm, calculating the average absorbance values of UVC (200-290 nm), UVB (290-320 nm) and UVA (320-400 nm), and comparing the ultraviolet absorption capacity, wherein the results are shown in Table 3.

TABLE 3 influence of the ratio of eaglewood leaf powder to extraction solvent feed liquid on sunscreen activity of eaglewood leaf extract

As can be seen from Table 3, the ratio of eaglewood leaf powder to 40% (by volume) of the alkaline ethanol solution was from 0.20: 45(g/mL) to 1.00: 45(g/mL), the average absorbance of the extract of eaglewood leaves becomes greater as the concentration increases, but when the feed-to-liquid ratio is 1.00: after 45(g/mL), the absorbance showed a tendency to decrease. The reduction is not obvious, but when the feed-liquid ratio is 0.80: after 45(g/mL), the increase in absorbance was not significant, at a feed-to-liquid ratio of 1.00: when the concentration is 45(g/mL), the average absorbance of the eaglewood leaf extracting solution reaches the highest peak, and the material-liquid ratio is 1.00: at 45(g/mL), the sunscreen active substances in the agilawood leaves are completely extracted, the material-liquid ratio is increased, the average absorbance of the extracting solution is not increased, and the waste of raw materials is caused, so that the optimal material-liquid ratio is 1.00: 45 (g/mL).

4) Influence of ultrasonic time on sunscreen activity of agilawood leaf extracting solution

According to the extraction method, 40 percent (volume) of alkaline ethanol solution is used as an extraction solvent, and the ratio of material to liquid is 1.00: 45 (g. mL)^-1) Changing the ultrasonic reflux time to 30, 50, 70, 90, 110 and 130min respectively under the conditions that the extraction temperature is 70 ℃, the ultrasonic power is 80W and the frequency is 80KHz is not changed, carrying out suction filtration, collecting filtrate, carrying out constant volume by using 40 percent (volume) alkaline ethanol solution, measuring the absorbance of the extracting solution in the wavelength range of 200-400 nm, calculating the average absorbance values of UVC (200-290 nm), UVB (290-320 nm) and UVA (320-400 nm), comparing the ultraviolet absorption capacity, and selecting the optimal extraction time. The sun protection ability was compared. The results are shown in Table 4.

TABLE 4 Effect of extraction time on sunscreen Activity of extract of Aquilaria sinensis

As can be seen from Table 4, the peak value of the sum of the average absorbances of the eaglewood leaf extracting solution to ultraviolet rays with wave bands of UVA (320-400 nm) and UVB (290-320 nm) appears in 50min, and the sum of the average absorbances of the eaglewood leaf extracting solution does not rise but shows a descending trend after the extraction time exceeds 50 min. It follows that the longer the extraction time is, the better the extraction is, since the longer the extraction time is, the more unstable sunscreen components in the extract are decomposed, which results in an undesirable effect of the final extract. Therefore, 50min was determined as the optimal extraction time.

5) Effect of Power on sunscreen Activity of extract of Aquilaria sinensis

According to the extraction method, 40 percent (volume) of alkaline ethanol solution is used as an extraction solvent, and the ratio of material to liquid is 1.0: 45 (g. mL)^－1) Changing ultrasonic power to 60W, 80W, 100W, 120W, 140W, 160W and 180W respectively under the conditions of extraction temperature of 70 ℃, extraction time of 50min and frequency of 80KHz unchanged, performing suction filtration after extraction is finished, collecting filtrate, fixing the volume of the filtrate by using 40 percent (volume) alkaline ethanol solution, measuring the absorbance of the extract in the wavelength range of 200-400 nm, and calculating the UVC (200-290 nm), UVB (290-320 nm) and UV (ultraviolet) of the extractThe average absorbance values of A (320-400 nm) are shown in Table 5 for comparison of the ultraviolet absorption capacity.

TABLE 5 Effect of extraction Power on sunscreen Activity of extract of Aquilaria sinensis

As can be seen from Table 5, the power has little influence on the extraction of the agilawood leaf sunscreen components, the absorbance of the extract liquid reaches the highest when the power is 80W, and the extraction efficiency is not increased when the power is increased. On the contrary, with the increase of the ultrasonic power, the solvent rapidly enters the eaglewood leaf sample, and the functional components are dissolved in the solvent as completely as possible to obtain a multi-component mixed extracting solution, so that the dissolution of the sunscreen components is influenced, and the content of the effective sunscreen components is reduced. Therefore, the optimum extraction power of ultrasound is 80W.

6) Influence of temperature on sunscreen activity of extractive solution

According to the extraction method, 40 percent (volume) of alkaline ethanol solution is used as an extraction solvent, and the ratio of the material to the liquid is kept between 1.0: 45 (g. mL)^-1) Under the condition that the conditions of extraction time is 50min, ultrasonic power is 80W, frequency is 80KHz and the like are not changed, ultrasonic extraction is carried out at the extraction temperatures of 30, 40, 50, 60, 70 and 80 ℃, suction filtration is carried out after extraction is finished, filtrate is collected, the volume is fixed by 40 percent (volume) alkaline ethanol solution, the absorbance of the extracting solution in the wavelength range of 200-400 nm is measured, the average absorbance values of UVC (200-290 nm), UVB (290-320 nm) and UVA (320-400 nm) are calculated, the ultraviolet absorption capacity is compared, and the optimal extraction temperature is selected. The results are shown in Table 6.

TABLE 6 Effect of temperature on sunscreen Activity of extract of Aquilaria sinensis

As can be seen from Table 6, the extract obtained at an extraction temperature of 80 ℃ has a good absorbance against ultraviolet rays in the UVA band range; the extract obtained at 70 deg.C has good absorption of ultraviolet rays with wavelength of UVB (290-320 nm) and UVC (200-290 nm). The absorbance of the extract obtained at 30 ℃ and 40 ℃ tends to increase, and the absorbance of the extract at 50 ℃ to 70 ℃ also tends to increase. In general, the temperature of 70 ℃ can sufficiently extract the sunscreen active, and the efficacy substances in the agilawood leaves can not be decomposed due to the high temperature. Therefore, the optimum extraction temperature is 70 ℃.

Example 1

Picking and collecting the agilawood leaves, cleaning, naturally drying, crushing the dried agilawood leaves, sieving with a 100-mesh sieve, weighing agilawood leaf powder 10g, adding 300ml of 40% (volume) alkaline ethanol solution, and performing ultrasonic-assisted extraction twice; the ultrasonic conditions are as follows: the ultrasonic power is 120W, and the frequency is 25 kHz; the extraction temperature is 70 deg.C, and the extraction time is 50 min/time; filtering after extraction is finished, collecting and combining filtrate, recovering ethanol, and concentrating under reduced pressure at 60 ℃ until no alcohol smell is produced to obtain 1.83g of extract which is marked as eaglewood leaf extract 1.

Example 2

Picking and collecting the agilawood leaves, cleaning, naturally drying, crushing the dried agilawood leaves, sieving with a 100-mesh sieve, weighing agilawood leaf powder 10g, adding 450ml of 40% (volume) alkaline ethanol solution, and performing ultrasonic-assisted extraction twice; the ultrasonic conditions are as follows: the ultrasonic power is 120W, and the frequency is 25 kHz; the extraction temperature is 70 deg.C, and the extraction time is 50 min/time; filtering after extraction is finished, collecting and combining filtrate, recovering ethanol, and concentrating under reduced pressure at 60 ℃ until no alcohol smell is produced to obtain 2.02g of extract, which is recorded as eaglewood leaf extract 2.

Example 3

Picking and collecting the agilawood leaves, cleaning, naturally drying, crushing the dried agilawood leaves, sieving with a 100-mesh sieve, weighing agilawood leaf powder 10g, adding 600ml of 40% (volume) alkaline ethanol solution, and performing ultrasonic-assisted extraction twice; the ultrasonic conditions are as follows: the ultrasonic power is 120W, and the frequency is 25 kHz; the extraction temperature is 70 deg.C, and the extraction time is 50 min/time; filtering after extraction is finished, collecting and combining filtrate, recovering ethanol, and concentrating under reduced pressure at 60 ℃ until no alcohol smell is produced to obtain 1.96g of extract which is recorded as eaglewood leaf extract 3.

Example 4

Picking and collecting the agilawood leaves, cleaning, naturally drying, crushing the dried agilawood leaves, sieving with a 100-mesh sieve, weighing agilawood leaf powder 10g, adding 450ml of 40% (volume) alkaline ethanol solution, and performing ultrasonic-assisted extraction for 2 times; the ultrasonic conditions are as follows: the ultrasonic power is 80W, and the frequency is 25 kHz; the extraction temperature is 50 deg.C, and the extraction time is 50 min/time; filtering after extraction is finished, collecting and combining filtrate, and concentrating under reduced pressure at 60 ℃ until no alcohol smell exists to obtain 1.82g of extract which is marked as the agilawood leaf extract 4.

Example 5

Picking and collecting the agilawood leaves, cleaning, naturally drying, crushing the dried agilawood leaves, sieving with a 100-mesh sieve, weighing agilawood leaf powder 10g, adding 450ml of 40% (volume) alkaline ethanol solution, and performing ultrasonic-assisted extraction for 2 times; the ultrasonic conditions are as follows: the ultrasonic power is 120W, and the frequency is 25 kHz; the extraction temperature is 50 deg.C, and the extraction time is 50 min/time; filtering after extraction, collecting and combining filtrates, recovering ethanol, and concentrating under reduced pressure at 60 deg.C until no ethanol smell is obtained to obtain extract 1.86g, which is recorded as eaglewood leaf extract 5.

Example 6

Picking and collecting the agilawood leaves, cleaning, naturally drying, crushing the dried agilawood leaves, sieving with a 100-mesh sieve, weighing agilawood leaf powder 10g, adding 450ml of 40% (volume) alkaline ethanol solution, and performing ultrasonic-assisted extraction twice; the ultrasonic conditions are as follows: ultrasonic power 160W, frequency 25 kHz; the extraction temperature is 50 deg.C, and the extraction time is 70 min/time; filtering after extraction is finished, collecting and combining filtrate, recovering ethanol, and concentrating under reduced pressure at 60 ℃ until no alcohol smell exists to obtain extract 1.88g which is recorded as agilawood leaf extract 6.

The method for evaluating the ultraviolet absorption effect of the agilawood leaf extract provided by the embodiment of the invention comprises the following steps:

1. preparation of the test specimens

0.05g of each eaglewood leaf extract in the embodiment is accurately weighed and dissolved in 100ml of absolute ethyl alcohol respectively to prepare eaglewood leaf extract solution of 0.50 g/L. A0.50 g/L solution of benzophenone-3 (BP-3) and Octyl Methoxycinnamate (OMC) were then prepared and subjected to a UV absorbance test to record absorbance values, the results of which are shown in Table 7.

TABLE 7 comparison of UV absorption of the extract of Aquilaria sinensis with other common sunscreens

2. Determination of the sun protection factor SPF:

sun Protection Factor (SPF): the ratio of the MED required to cause erythema on skin protected by sunscreen to the MED required to cause erythema on unprotected skin is the SPF of the sunscreen.

According to the standard preparation method of the sunscreen cosmetic, the agilawood leaf extract prepared in the example 2 is added into the base material of the sunscreen cosmetic according to the proportion range of 1-10%, and the specific formula proportion is shown in table 8.

TABLE 8 formula of sunscreen cream containing folium Pelargonii Graveolentis extract

Respectively heating the phase A and the phase B in the table 8 to 72-82 ℃, and continuously stirring until all the components are dissolved. Adding the phase A into the phase B while stirring, and continuing stirring until the formed emulsion is cooled to room temperature (15-30 ℃) so as to obtain 100g of a sun-proof sample. The sun protection factor SPF of the sunscreen cosmetic was then determined as specified in technical specifications for cosmetic safety (2015), and the results are shown in table 9.

Table 9 agilawood leaf extract sunscreen cream SPF value test results

3. Tyrosinase inhibitory activity effect evaluation test

0.05g of each eaglewood leaf extract in the embodiment is accurately weighed and dissolved in 100ml of absolute ethyl alcohol respectively to prepare eaglewood leaf extract solution of 0.50 g/L. Accurately sucking a sample solution (0.50g/L of the eaglewood leaf extract solution), a Phosphate Buffer Solution (PBS) with the pH value of 6.86 and an L-tyrosine solution according to the table 10, fully mixing, culturing in a water bath at 37 ℃ for 10min at constant temperature, adding the required L-tyrosinase solution, reacting in the water bath at 37 ℃ for 10min, and measuring the absorbance at 475 nm. Vitamin C and arbutin are used as reference substances.

TABLE 10 composition of tyrosinase activity inhibition test reaction System

Tyrosinase inhibition (%) ([ 1- (T)₂-T₁)/(C₂-C₁)]X 100% where C₁Absorbance of neither sample solution nor enzyme solution, C₂The absorbance of the enzyme solution added to the sample is not added; t is₁Absorbance of the solution with sample and without enzyme, T₂The absorbance of the sample solution and the enzyme solution was measured.

TABLE 11 tyrosinase inhibition assay results for eaglewood leaf extract

Remarking: under the same conditions, the tyrosinase inhibition rates of vitamin C and arbutin are 52.6% and 61.5%, respectively.

4. Evaluation test of superoxide anion radical scavenging effect

(1) Accurately weighing the extract of the agilawood leaves in the example 2, dissolving the extract in 100ml of absolute ethyl alcohol, and preparing sample solutions with mass concentrations of 100, 200, 300, 400 and 500mg/L respectively.

(2) Respectively adding 4ml (0.05mol/L) of Tris-HCl buffer solution with pH of 8.2 into a 10ml colorimetric tube, preheating for 20min in a water bath at 25 ℃, then adding 1ml of sample solutions with different concentrations, then adding 1ml of 0.2mmol/L pyrogallol solution preheated for 20min in the water bath at 25 ℃, reacting for 4min in the water bath at 25 ℃ after uniformly mixing, standingThe reaction was terminated in two drops with concentrated HCl and the absorbance (A) was measured at a wavelength of 325nm_{Sample (A)}). Each tube was repeated three times and averaged.

In the above procedure, only 1ml of distilled water was used in place of the sample solution, and the result was determined as the original tube (A)_{Original source}). Each tube was repeated three times and averaged.

The results were calculated as follows:

O₂ ^-clearance (%) ═ a_{Original source}-A_{Sample (A)})/A_{Original source}×100％

The results of the superoxide anion radical scavenging effect are shown in Table 12.

TABLE 12 Dermatopanax leaf extract superoxide anion radical scavenging test results (100%)

The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.