CN108324603B - A cosmetic containing pollen Pini extract and its preparation method - Google Patents

Abstract

The invention belongs to the technical field of biology, and particularly relates to a cosmetic containing a pine pollen extract and a preparation process thereof. According to the invention, the method of ethanol extraction and ethanol precipitation is adopted to extract the pine pollen, so that the problem of fine precipitate generation in the pine pollen extract is solved, and the stable pine pollen extract is obtained; the invention uses proper macroporous absorption resin to refine and purify the flavone; the concentrated solution is blended by using a polyalcohol aqueous solution to form the pine pollen extract taking the polyalcohol aqueous solution as a system, and the obtained extract is stable, has good compatibility with cosmetics and small irritation to skin, and provides a foundation for applying the pine pollen extract to the field of cosmetics. The method for extracting the pine pollen has the advantages of simple process, high yield, less impurities and strong operability, the obtained pine pollen extract has good stability, no precipitate is generated, the allergy risk is low, the pine pollen extract has good compatibility with cosmetic matrixes, and the obtained cosmetics have the effects of whitening, resisting aging, resisting bacteria and resisting inflammation.

Description

A cosmetic containing pollen Pini extract and its preparation method

Technical Field

The invention belongs to the technical field of biology, and particularly relates to a cosmetic containing a pine pollen extract and a preparation process thereof.

Background

Since ancient pine pollen is a treasure for food therapy and beauty treatment, the application of the ancient pine pollen on skin care products has a long history, and the pine pollen recorded in Qing 'materia medica-Yao Xin' records that the pine pollen is good in broken grains and sores and does not scab when being wet. Modern scientific research shows that the pine pollen contains various nutrient components such as vitamins, proteins, amino acids, fat and the like, and is known as a super micro nutrient bank. The pollen flavone and other active components have whitening, anti-aging, antibacterial and anti-inflammatory effects, and are often used in cosmetics.

In the prior several flavone extraction processes, the hot water extraction method has more impurities and low yield; the alkali extraction and acid precipitation method is not feasible for extracting the pollen pini flavone, and the addition of acid is found to be incapable of effectively precipitating after the attempt; the supercritical extraction cost is too high; the enzyme extraction method and the alcohol extraction method have simple and easy processes, high yield and less impurities, but after the attempt, the system can generate fine particles continuously, and the problem of passing through a microporous membrane cannot be solved.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a cosmetic containing a pine pollen extract and a preparation process thereof.

The invention provides a cosmetic containing a pine pollen extract, which comprises the following components in percentage by weight: 50-60% of water, 3-8% of glycerol, 3-8% of 1, 3-butanediol, 0.3-3% of nicotinamide, 3-8% of pine pollen extract, 1-5% of octadecanol, 3-7% of D-panthenol, 3-8% of caprylic/capric triglyceride, 3-8% of synthetic squalane, 1-4% of silicone oil 200, 1-5% of jojoba oil, 0.5-2% of PMX-0345 silicone oil, 0.5-1% of phenoxyethanol, 2-6% of Tween-60 and 2-6% of NIKKOL NikkomuseSE.

The preparation process of the pine pollen extract comprises the following steps:

(1) alcohol extraction: adding 25-95 wt% ethanol into pollen Pini, and extracting under reflux at 40-1000W, 10-70KHz and 10-99 deg.C under assistance of ultrasound for 1-3 hr to obtain extractive solution; wherein, the weight ratio of the ethanol to the pine pollen is (1-100) to 1;

(2) and (3) filtering and concentrating: filtering the extracting solution in the step (1) while the extracting solution is hot, and concentrating the obtained filtrate under reduced pressure at the temperature of 10-90 ℃ until the liquid is in an extract state;

(3) alcohol precipitation: cooling the concentrated solution obtained in the step (2) to-10 ℃, adding 75-99.9 wt% ethanol with the concentration being 1-5 times of the weight of the concentrated solution, stirring for 1-40min, and standing for alcohol precipitation for 1-20 h;

(4) and (3) filtering: filtering the alcohol precipitation filtrate obtained in the step (3) through a 0.22-10 mu m microporous membrane, and collecting the filtrate;

(5) resin purification: adsorbing flavone in the filtrate obtained in the step (4) by adopting AB-8 macroporous adsorption resin, wherein the weight of the adsorption resin is 1-20 times that of the filtrate, and the adsorption flow rate is 1-10 BV/h; eluting with purified water 1-10 times the volume of the adsorbent resin at a flow rate of 1-10 BV/h; finally, eluting with 50-99.5 wt% ethanol with the volume 1-20 times that of the adsorption resin at the flow rate of 1-15 BV/h;

(6) concentration: concentrating the liquid purified by the resin in the step (5) at 10-90 ℃ under reduced pressure until the liquid is in an extract state;

(7) and (4) taking the concentrated solution obtained in the step (6), adding 1, 3-butanediol with the weight 1-16 times of that of the concentrated solution and purified water with the weight 1-10 times of that of the concentrated solution, and adding MTI with the weight 0.02 time of that of the concentrated solution to obtain the pine pollen extract.

Wherein the NIKKOL Nikkomulse SE is purchased from Sun chemical commerce (Shanghai) Inc.

The second purpose of the invention is to provide a preparation method of the cosmetic, which comprises the following steps:

(1) placing octadecanol, caprylic/capric acid glycerate, synthetic squalane, silicone oil-200, jojoba oil, PMX-0345 silicone oil, and tween-60 in an oil phase pan, heating to 80 deg.C, maintaining the temperature, and stirring for 30 min;

(2) heating glycerol, 1, 3-butanediol, nicotinamide, NIKKOL Nikkomule SE, and water in water phase pot to 80 deg.C, maintaining the temperature, and stirring for 30 min;

(3) slowly adding the materials in the water phase pot into the oil phase pot, stirring for 5min, and homogenizing for 5 min;

(4) stirring, cooling to below 45 deg.C, adding D-panthenol, pollen Pini extract and phenoxyethanol, and stirring for 30 min.

The invention has the beneficial effects that:

1. according to the invention, the method of ethanol extraction and ethanol precipitation is adopted to extract the pine pollen, so that the problem of fine precipitate generation in the pine pollen extract is solved, and the stable pine pollen extract is obtained; the invention uses proper macroporous absorption resin to refine and purify the flavone; the concentrated solution is blended by using a polyalcohol aqueous solution to form the pine pollen extract taking the polyalcohol aqueous solution as a system, and the obtained extract is stable, has good compatibility with cosmetics and small irritation to skin, and provides a foundation for applying the pine pollen extract to the field of cosmetics.

2. The method for extracting the pine pollen has the advantages of simple process, high yield, less impurities and strong operability, the obtained pine pollen extract has good stability, no precipitate is generated, the allergy risk is low, the pine pollen extract has good compatibility with cosmetic matrixes, and the obtained cosmetics have the effects of whitening, resisting aging, resisting bacteria and resisting inflammation.

Drawings

FIG. 1 is a schematic diagram of DPPH free radical scavenging rate of a pollen Pini extract prepared in example 1-2 of the present invention;

FIG. 2 is a graph showing the effect of pollen Pini extract at different concentrations on fibroblast survival rate;

FIG. 3 is a graph showing the R2 value of the skin elasticity of volunteers after applying the cosmetic.

Detailed Description

The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.

Example 1

A cosmetic containing pine pollen extract comprises the following components in percentage by weight: 52% of water, 5% of glycerol, 5% of 1, 3-butanediol, 1% of nicotinamide, 5% of a pine pollen extract, 3% of octadecanol, 5% of D-panthenol, 5% of caprylic/capric triglyceride, 5% of synthetic squalane, 2% of silicone oil 200, 3% of jojoba oil, 1% of PMX-0345 silicone oil, 1% of phenoxyethanol, 4% of tween-60 and 3% of NIKKOL Nikkomulese.

The preparation process of the pine pollen extract comprises the following steps:

(1) alcohol extraction: adding 75 wt% ethanol into pollen Pini, reflux-extracting in 85 deg.C water bath for 3 hr, and extracting for 2 times to obtain extractive solution; wherein the weight ratio of the ethanol to the pine pollen is 20: 1;

(2) and (3) filtering and concentrating: filtering the extracting solution in the step (1) while the extracting solution is hot, and concentrating the obtained filtrate under reduced pressure at 45 ℃ until the liquid is in an extract state;

(3) alcohol precipitation: cooling the concentrated solution obtained in the step (2) to 0 ℃, adding 95 wt% ethanol with the concentration 2.5 times of the weight of the concentrated solution, stirring for 5min, standing and precipitating with ethanol for 12 h;

(4) and (3) filtering: filtering the alcohol precipitation filtrate obtained in the step (3) through a 0.45-micrometer microporous membrane, and collecting the filtrate;

(5) resin purification: adsorbing flavone in the filtrate obtained in the step (4) by adopting AB-8 macroporous adsorption resin, wherein the weight of the adsorption resin is 6 times that of the filtrate, and the adsorption flow rate is 2 BV/h; then purified water with 5 times volume of the adsorption resin is adopted for elution, and the flow rate is 2 BV/h; finally, eluting by using 95 wt% ethanol with the volume 8 times that of the adsorption resin, wherein the flow rate is 5 BV/h;

(6) concentration: concentrating the liquid purified by the resin in the step (5) at 45 ℃ under reduced pressure to obtain an extract;

(7) and (4) taking the concentrated solution obtained in the step (6), adding 16 times of 1, 3-butanediol and 3 times of purified water, and adding MTI (methyl thiazolyl tetrazolium) in an amount which is 0.02 times of the weight of the concentrated solution to obtain a pollen pini extract, wherein the content of flavone is detected to be 0.20 mg/mL.

Example 2

A cosmetic containing pine pollen extract comprises the following components in percentage by weight: 57% water, 3% glycerol, 3% 1, 3-butylene glycol, 2% nicotinamide, 4% pollen pini extract, 5% octadecanol, 3% D-panthenol, 6% caprylic/capric triglyceride, 3% synthetic squalane, 1% silicone oil 200, 1% jojoba oil, 2% PMX-0345 silicone oil, 1% phenoxyethanol, 6% Tween-60 and 3% NIKKOL Nikkomulese.

The preparation process of the pine pollen extract comprises the following steps:

(1) alcohol extraction: adding 75 wt% ethanol into pollen Pini, and performing ultrasonic-assisted reflux extraction at 40W, 40KHz and 45 deg.C for 2h to obtain extractive solution; wherein the weight ratio of the ethanol to the pine pollen is 30: 1;

(2) and (3) filtering and concentrating: filtering the extracting solution in the step (1) while the extracting solution is hot, and concentrating the obtained filtrate under reduced pressure at the temperature of 60 ℃ until the liquid is in an extract state;

(3) alcohol precipitation: cooling the concentrated solution obtained in the step (2) to 4 ℃, adding 95 wt% ethanol with the weight 3.5 times that of the concentrated solution, stirring for 5min, standing and precipitating with ethanol for 12 h;

(4) and (3) filtering: filtering the alcohol precipitation filtrate obtained in the step (3) through a 0.45-micrometer microporous membrane, and collecting the filtrate;

(5) resin purification: adsorbing flavone in the filtrate obtained in the step (4) by adopting AB-8 macroporous adsorption resin, wherein the weight of the adsorption resin is 6 times that of the filtrate, and the adsorption flow rate is 2 BV/h; then purified water with 5 times volume of the adsorption resin is adopted for elution, and the flow rate is 2 BV/h; finally, eluting by using 95 wt% ethanol with the volume 8 times that of the adsorption resin, wherein the flow rate is 5 BV/h;

(6) concentration: concentrating the liquid purified by the resin in the step (5) at 45 ℃ under reduced pressure to obtain an extract;

(7) and (4) taking the concentrated solution obtained in the step (6), adding 1, 3-butanediol with the weight 12 times that of the concentrated solution and purified water with the weight 2 times that of the concentrated solution, and adding MTI with the weight 0.02 times that of the concentrated solution to obtain a pollen pini extract, wherein the content of flavone is detected to be 0.40 mg/mL.

Stability survey

The pollen pini extracts of the embodiments 1-2 are respectively taken 40g, averagely divided into four transparent sample bottles, placed in different environments, and the states are regularly observed. The four samples are respectively placed in an indoor sunshine irradiation place for 35 days, a 45 ℃ constant temperature box for 30 days, a-20 ℃ refrigerator freezing chamber for 7 days, a 45 ℃ constant temperature box and a-20 ℃ refrigerator freezing chamber for circulation and placement for 10 days. The state of the pine pollen extract is observed every day, the appearance change is extremely small, and the flavone content is almost unchanged, which indicates that the pine pollen extract has good stability.

Whitening and anti-aging efficacy evaluation

Table 1 shows the effect of the samples on the amount of melanin in B16 cells, and Table 2 shows the effect of the samples on the amount of tyrosinase activity in B16 cells.

TABLE 1

Sample name	Final concentration	A475±SD	Relative melanin content (%)
				cell only	-	0.116±0.001	100.0±9.3
8-mop	100uM	0.127±0.002	110.2±1.4
				Arbutin	10ug/mL	0.099±0.003	85.1±2.6
Pollen Pini extract-example 1	0.20mg/mL (flavone content)	0.089±0.002	78.1±1.7
				Pollen Pini extract-example 2	0.40mg/mL (flavone content)	0.078±0.009	69.9±0.8

TABLE 2

Sample name	Final concentration	A475±SD	Relative tyrosinase Activity (%)
				cell only	-	0.083±0.001	100.0±2.9
8-mop	100μM	0.104±0.002	149.4±10.6
				Arbutin	10ug/mL	0.078±0.002	78.9±5.2
Pollen Pini extract-example 1	0.20mg/mL (flavone content)	0.069±0.004	66.7±3.3
				Pollen Pini extract-example 2	0.40mg/mL (flavone content)	0.062±0.001	62.4±1.3

As shown in the data in tables 1 and 2, the pine pollen extract can inhibit tyrosinase activity, reduce melanin content, and has whitening effect.

TABLE 3 Effect of samples on the relative survival of fibroblasts

As can be seen from table 3, fig. 1 (fig. 1 shows the hydroxyl radical scavenging rates of example 1 and example 2 in sequence from left to right), and fig. 2 show that the pollen pini extract has a strong ability to scavenge hydroxyl radicals, and has a good effect of promoting the growth of fibroblasts. Fibroblasts, also called fibroblasts, are the main cell components of loose connective tissues and belong to terminally differentiated cells, and the cells can produce proteins such as collagen, thereby fully indicating the potential of the pine pollen extract possibly having the effect of inhibiting skin aging.

Evaluation of anti-aging efficacy of cosmetic

Skin elasticity measurement

The product was tried and used for measuring skin elasticity (R2 value) after 2 weeks, 4 weeks, 6 weeks, and 8 weeks using a skin elasticity tester.

Table 4 skin elasticity R2 values after use of the product

As can be seen from Table 4 and FIG. 3, the skin elasticity was improved to some extent by using the cosmetic, and the R2 value of the skin elasticity increased by 7.8% in the eighth week, which is of very significant statistical significance. The skin elasticity is an important index of the skin aging degree, which shows that the product has the effects of improving the skin elasticity, reducing wrinkles and slowing down the aging.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (2)

1. A cosmetic containing a pine pollen extract is characterized by comprising the following components in percentage by weight: 57% water, 3% glycerol, 3% 1, 3-butylene glycol, 2% nicotinamide, 4% pollen pini extract, 5% octadecanol, 3% D-panthenol, 6% caprylic/capric triglyceride, 3% synthetic squalane, 1% silicone oil 200, 1% jojoba oil, 2% PMX-0345 silicone oil, 1% phenoxyethanol, 6% tween-60, and 3% NIKKOL Nikkomulese;

the preparation process of the pine pollen extract comprises the following steps:

(1) alcohol extraction: adding 75 wt% ethanol into pollen Pini, and performing ultrasonic-assisted reflux extraction at 40W, 40KHz and 45 deg.C for 2h to obtain extractive solution; wherein the weight ratio of the ethanol to the pine pollen is 30: 1;

(2) and (3) filtering and concentrating: filtering the extracting solution in the step (1) while the extracting solution is hot, and concentrating the obtained filtrate under reduced pressure at the temperature of 60 ℃ until the liquid is in an extract state;

(3) alcohol precipitation: cooling the concentrated solution obtained in the step (2) to 4 ℃, adding 95 wt% ethanol with the weight 3.5 times that of the concentrated solution, stirring for 5min, standing and precipitating with ethanol for 12 h;

(4) and (3) filtering: filtering the alcohol precipitation filtrate obtained in the step (3) through a 0.45-micrometer microporous membrane, and collecting the filtrate;

(5) resin purification: adsorbing flavone in the filtrate obtained in the step (4) by adopting AB-8 macroporous adsorption resin, wherein the weight of the adsorption resin is 6 times that of the filtrate, and the adsorption flow rate is 2 BV/h; then purified water with 5 times volume of the adsorption resin is adopted for elution, and the flow rate is 2 BV/h; finally, eluting by using 95 wt% ethanol with the volume 8 times that of the adsorption resin, wherein the flow rate is 5 BV/h;

(6) concentration: concentrating the liquid purified by the resin in the step (5) at 45 ℃ under reduced pressure to obtain an extract;

(7) and (4) taking the concentrated solution obtained in the step (6), adding 1, 3-butanediol with the weight 12 times that of the concentrated solution and purified water with the weight 2 times that of the concentrated solution, and adding MTI with the weight 0.02 times that of the concentrated solution to obtain a pollen pini extract, wherein the content of flavone is detected to be 0.40 mg/mL.

2. A method for preparing the cosmetic of claim 1, comprising the steps of:

(1) placing octadecanol, caprylic/capric acid glycerate, synthetic squalane, silicone oil-200, jojoba oil, PMX-0345 silicone oil, and tween-60 in an oil phase pan, heating to 80 deg.C, maintaining the temperature, and stirring for 30 min;

(2) heating glycerol, 1, 3-butanediol, nicotinamide, NIKKOL Nikkomule SE, and water in water phase pot to 80 deg.C, maintaining the temperature, and stirring for 30 min;

(3) slowly adding the materials in the water phase pot into the oil phase pot, stirring for 5min, and homogenizing for 5 min;

(4) stirring, cooling to below 45 deg.C, adding D-panthenol, pollen Pini extract and phenoxyethanol, and stirring for 30 min.

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