阅读说明：本技术 一种应用于化妆品的海藻抗炎提取物的制备方法 (Preparation method of seaweed anti-inflammatory extract applied to cosmetics ) 是由 邹鹏飞 于建伟 赵乐荣 牟维林 陶宇 唐文金 卢伟超 于 2019-11-12 设计创作，主要内容包括：本发明提供了一种新的海藻抗炎提取物的制备方法,提高小分子海带提取物中岩藻聚糖硫酸酯的透皮效果,从而有助于其在抗炎类化妆品中的应用。发明包括如下步骤：(1)水提法提取海带粗多糖；(2)高压脉冲电场处理步骤(1)获得的海带粗多糖溶液；(3)步骤(2)获得的粗多糖用过氧化氢法裂解；(4)通过滤膜处理,脱除杂质并保留所需的分子量范围。本发明通过对富含岩藻聚糖硫酸酯的海带水提取物进行特定的高压脉冲电场处理,有效提高了其裂解产物中岩藻聚糖硫酸酯的透皮效果,解决了传统小分子海带提取物透皮效果不理想的问题。本发明不使用促炎、对皮肤有不良影响的透皮促进剂,使化妆品成分更加安全。(The invention provides a novel preparation method of a seaweed anti-inflammatory extract, which improves the transdermal effect of fucosan sulfate in a micromolecular seaweed extract, thereby being beneficial to the application of the seaweed anti-inflammatory extract in anti-inflammatory cosmetics. The invention comprises the following steps: (1) extracting crude polysaccharide from herba Zosterae Marinae with water; (2) treating the crude kelp polysaccharide solution obtained in the step (1) by using a high-voltage pulse electric field; (3) cracking the crude polysaccharide obtained in the step (2) by using a hydrogen peroxide method; (4) through the membrane treatment, impurities are removed and the desired molecular weight range is retained. The invention effectively improves the transdermal effect of fucosan sulfate in the cracking product of the kelp water extract by carrying out specific high-voltage pulse electric field treatment on the kelp water extract rich in fucosan sulfate, and solves the problem that the transdermal effect of the traditional micromolecule kelp extract is not ideal. The invention does not use a skin penetration enhancer which has proinflammatory effect and adverse effect on skin, so that the cosmetic ingredients are safer.)

1. A preparation method of seaweed anti-inflammatory extract applied to cosmetics is characterized by comprising the following steps:

(1) extracting crude polysaccharide from herba Zosterae Marinae with water;

(2) treating the crude kelp polysaccharide solution obtained in the step (1) by using a high-voltage pulse electric field; the working conditions of the high-voltage pulse electric field treatment are as follows: the electric field intensity is 10-20kV/cm, the pulse frequency is 50-150Hz, the pulse time is 80-160 mus, and the pulse width is 5-10 mus.

(3) Cracking the crude polysaccharide obtained in the step (2) by using a hydrogen peroxide method;

(4) and (4) carrying out filter membrane treatment on the lysate obtained in the step (3).

2. The method according to claim 1, wherein the operating conditions of step (1) are: soaking 80-200 mesh dry powder of herba Zosterae Marinae in water at a mass ratio of 1:20-1:50 for 10-24 hr; after soaking, leaching the reaction system in water bath at 45-90 ℃ for 2-24h, and centrifuging to obtain crude kelp polysaccharide solution.

3. The method according to claim 1, wherein the temperature of the crude laminarin solution of kelp in the step (2) is 35 to 45 ℃.

4. The working condition of the step (3) is that the crude polysaccharide solution of the kelp obtained in the step (2) is concentrated and dried to obtain crude polysaccharide powder; using hydrogen peroxide cracking method, the crude polysaccharide powder is 1-3 wt%, the hydrogen peroxide is 0.5-1.5 wt%, and the rest is water; the reaction temperature is 60-80 ℃, and the reaction time is 70-180 min.

5. The method according to claim 1, wherein the membrane treatment in step (4) is ultrafiltration comprising filtration using a membrane having a molecular weight cut-off of 1 to 3 kDa.

6. The method of claim 1, further comprising the step of formulating the product obtained in step (4) with a hyprolose oligosaccharide.

7. The method according to claim 6, wherein the molecular weight of the hyphostroma oligosaccharide is 500Da or less.

8. The method according to claim 6, wherein the product obtained in the step (4) is prepared into dry powder, and the mass ratio of the dry powder to the dried powder of the hypsizygus marmoreus oligosaccharide is 20:1-40: 1.

9. The method according to claim 6, wherein the polysaccharide is obtained by hydrogen peroxide decomposition.

Technical Field

The invention relates to a preparation method of a seaweed anti-inflammatory extract applied to cosmetics.

Background

The fucosan sulfate is a seaweed sulfated polysaccharide with high added value, has various biological activities, and has wide application prospect in the fields of medicines and cosmetics. Research shows that the fucoidan sulfate has obvious anti-inflammatory effect and has development potential in the aspects of hand washing gel, personal care products, cosmetics special for inflammatory skin and cosmetics special for sensitive skin. However, it has not been widely used in the cosmetic field.

Obtaining pure fucoidan sulfate usually requires a complicated purification process, is expensive to produce, and is difficult to avoid the use of organic reagents during the purification process, which affects the safety of the ingredients and increases the risk of introducing allergic substances into the system.

The fucoidan sulfate is mainly extracted from kelp, which is cheap and easily available, and most fucoidan sulfate can be extracted by hot water extraction; however, aqueous kelp extracts also contain a large number of impurities, including complex polysaccharide components. The kelp water extract is directly applied to cosmetic raw materials, and the transdermal effect is not ideal, so that the anti-inflammatory effect of the kelp water extract is influenced, and the application of the kelp water extract in cosmetics with anti-inflammatory effect is influenced.

The problem of transdermal absorption has been a prerequisite for the evaluation of cosmetic effectiveness. Anti-inflammatory cosmetics require relatively high transdermal performance, but the prior art generally increases transdermal performance by the addition of penetration enhancers. However, the transdermal agent is usually an organic acid or a surfactant, does not utilize the recovery of inflammation, even belongs to a proinflammatory substance, and is not suitable for the use of anti-inflammatory cosmetics.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a novel preparation method of the seaweed anti-inflammatory extract, which improves the transdermal effect of fucosan sulfate in the micromolecular seaweed extract, thereby being beneficial to the application of the seaweed anti-inflammatory extract in anti-inflammatory cosmetics.

A method for preparing antiinflammatory Sargassum extract for cosmetic comprises the following steps:

(1) extracting crude polysaccharide from herba Zosterae Marinae with water;

(2) treating the crude kelp polysaccharide solution obtained in the step (1) by using a high-voltage pulse electric field; the working conditions of the high-voltage pulse electric field treatment are as follows: the electric field intensity is 10-20kV/cm, the pulse frequency is 50-150Hz, and the pulse time is 80-160 mus.

(3) Cracking the crude polysaccharide obtained in the step (2) by using a hydrogen peroxide method;

(4) through the membrane treatment, impurities are removed and the desired molecular weight range is retained.

The high-voltage Pulse Electric Field (PEF) is a non-thermal processing technology for processing liquid food under conditions of high voltage, short pulse, mild temperature and the like, is first applied to the field of non-thermal processing of fruits and vegetables, and has recently become a research hotspot for processing liquid food. Under the condition of a high-voltage pulse electric field, water can be slightly ionized, the electrification condition of macromolecules in a system is influenced, and further the conformation is influenced. However, except for sterilization and improvement of extraction rate, other application mechanisms are not clear; its application range is also limited. The method is used for treating crude kelp polysaccharide, and the transdermal effect of fucosan sulfate in a lysate of the crude kelp polysaccharide is unexpectedly promoted, so that the transdermal absorption of an anti-inflammatory active substance fucosan sulfate is promoted.

It is to be noted that, in the step (1), the kelp raw material from which the crude kelp polysaccharide is extracted must be desalted in advance.

And (3) selecting a flowing type for the high-voltage pulse electric field device in the step (2). The treatment flow rate of the feed liquid is calculated from the parameters and the treatment chamber volume.

Preferably, the working conditions of the step (1) are as follows: soaking 80-200 mesh dry powder of herba Zosterae Marinae in water at a mass ratio of 1:20-1:50 for 10-24 hr; after soaking, leaching the reaction system in water bath at 45-90 ℃ for 2-24h, centrifuging, and taking supernatant to obtain crude kelp polysaccharide solution. The kelp dry powder is prepared from desalted kelp, and the content of soluble salt is lower than 2%. The desalting treatment can be rinsing desalting with clear water.

It should be noted that the high-pressure extraction method at a temperature of more than 100 ℃ can improve the yield to a small extent and produce a certain cracking effect, but the improvement of the transdermal effect after the treatment of the high-voltage pulse electric field is not obvious.

Preferably, the kelp extract obtained in step (1) is subjected to decolorization treatment, preferably macroporous resin decolorization, and activated carbon decolorization can also be used.

Preferably, the temperature of the crude laminarin solution of kelp is adjusted to 35-45 ℃ before step (2) is carried out.

Generally speaking, a high-voltage pulse electric field belongs to a non-thermal processing technology, is generally applied to a normal temperature condition, and rarely discusses the influence of the reaction temperature on the action effect. The invention finds that the proper temperature can bring better transdermal effect of the lysate, and the proper temperature range is slightly higher than the normal temperature.

Preferably, the working conditions of the step (3) are to concentrate and dry the crude kelp polysaccharide solution obtained in the step (2) to obtain crude polysaccharide powder; using hydrogen peroxide cracking method, the crude polysaccharide powder is 1-3 wt%, the hydrogen peroxide is 1-2.5 wt%, the rest is water, the reaction temperature is 60-80 deg.C, and the reaction time is 70-180 min.

The concentration can be rotary evaporation concentration or vacuum concentration, and the drying can be freeze drying or spray drying.

Preferably, the technical means of step (4) may be ultrafiltration or dialysis. The filter membrane can only remove small molecules and salt, and can also obtain substances in a target molecular weight range by filtering more than twice. The cut-off molecular weight of the desalting and small-molecule filter membrane is preferably 1-3 kDa.

After ultrafiltration, the obtained feed liquid is dried to obtain dry powder. The drying means may be freeze drying or spray drying.

Preferably, the kelp extract dry powder prepared by the method is mixed with the kelp oligosaccharide, and the mixture is uniformly mixed, wherein the mass ratio of the kelp extract to the kelp oligosaccharide is 20:1-40: 1.

Wherein the polysaccharide is obtained by extracting polysaccharide from Lacca deliciosa with water, splitting by hydrogen peroxide method, and drying, and has molecular weight below 500 Da.

The experimental result of the invention shows that the hyphostroma oligosaccharide is an effective fucosan sulfate penetration enhancer, and the hyphostroma oligosaccharide has the effects of moisture retention and antioxidation, thereby avoiding further deterioration of inflammation caused by organic acids and surface active penetration enhancers.

The hydrogen peroxide cracking method is that 1.5 wt% -3 wt% of the polysaccharide of the hypsizygus marmoreus, 2.5 wt% -5 wt% of hydrogen peroxide and the balance of water are cracked for 60-150min at 50-80 ℃ and ultrafiltered to obtain the hypsizygus marmoreus oligosaccharide below 500Da in a reaction system.

The invention has the following beneficial effects:

the invention effectively improves the transdermal effect of fucosan sulfate in the cracking product of the kelp water extract by carrying out specific high-voltage pulse electric field treatment on the kelp water extract rich in fucosan sulfate, and solves the problem that the transdermal effect of the traditional micromolecule kelp extract is not ideal. The invention does not need to separate and purify the fucosan sulfate, reduces the production cost, does not need to use an organic reagent, and is beneficial to the application of the fucosan sulfate in cosmetics and washing and caring products. The invention also combines the product with the hyphostroma oligosaccharide, and experiments prove that the hyphostroma oligosaccharide is an effective transdermal enhancer. The invention does not use a skin penetration enhancer which has proinflammatory effect and adverse effect on skin, so that the cosmetic ingredients are safer.

Drawings

FIG. 1 is a schematic view of a transdermal absorption experimental apparatus;

FIG. 2 is a graph showing the cumulative permeation amount per unit area as a function of time for example 2, Experimental example 1 and Experimental example 2;

FIG. 3 is a graph of the cumulative permeation per unit area as a function of time for Experimental example 3, example 1, example 2, and example 3;

in fig. 1: 1. a supply tank; 2. a sampling port; 3. a receiving pool; 4. and (4) stirring.

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.