CN114224802A

CN114224802A - Long-acting fresh-keeping skin-care type hydrolat based on natural traditional Chinese medicines and preparation method thereof

Info

Publication number: CN114224802A
Application number: CN202111678467.8A
Authority: CN
Inventors: 张嘉宁
Original assignee: Shanghai Zhiyong Education Training Co ltd
Current assignee: Shanghai Zhiyong Education Training Co ltd
Priority date: 2021-12-31
Filing date: 2021-12-31
Publication date: 2022-03-25

Abstract

The long-acting fresh-keeping hydrolat comprises plant source hydrolat stock solution and bacteriostatic traditional Chinese medicinal materials, wherein the bacteriostatic traditional Chinese medicinal materials are selected from one or more of folium artemisiae argyi, honeysuckle, pepper, semen cassiae, fennel and litsea cubeba.

Description

Long-acting fresh-keeping skin-care type hydrolat based on natural traditional Chinese medicines and preparation method thereof

Technical Field

The invention relates to the technical field of skin care, in particular to a long-acting fresh-keeping skin-care type hydrolat based on natural traditional Chinese medicines and a preparation method thereof.

Background

The hydrolat extracted from plants contains all water-soluble substances in plants, such as tannin and flavonoid, and is more easily absorbed by skin than essential oil. However, the preservation time of the hydrolat is short, the hydrolat which is not opened can be preserved for 1-2 years at normal temperature, and the hydrolat can be preserved for about one quarter after the cover is opened, and the hydrolat will deteriorate.

Because of the change of storage environment such as temperature, humidity, illumination etc., nutrient substances such as amino acid, polypeptide in the pure dew will be separated out, form white floccule, it is apt to cause allergic symptoms when being smeared on the skin.

In cosmetic products, compared with products synthesized by chemical engineering, skin care products extracted from pure nature are very popular with female consumers, and hydrolat is a pure natural plant extract, and can be used for preparing various facial masks or used as a moisturizing skin care product. However, the pure dew is short in storage time, the ordinary unopened pure dew can be stored for 1-2 years at normal temperature, and generally only can be placed for about one quarter after the pure dew is opened, so that the natural extract is added into the high-activity pure dew to improve the antibacterial and antioxidant capacity of the high-activity pure dew, and therefore the storage time of the high-activity pure dew is prolonged, and the high-activity pure dew is a development trend of a pure dew quality guarantee process.

In the existing methods for refreshing and improving the activity of rose hydrosol, the royal and the like (2020) prove that the ratio of flower liquid to rose hydrosol is 1: 1.7 g/mL in the research of the optimization of the extraction process of the rose hydrosol and the antibacterial activity^-1Under the conditions that the reflux time is 7min and the distillation temperature is 120 ℃, the obtained hydrolat has the highest sensory score; under the condition, the clearance rate of DPPH & superoxide anion of the rose hydrosol extracted under the condition is 24.66 percent and 5.03 percent respectively. (northern horticulture 2020(18): 106-. Studies on the extraction of plant hydrolat and its antibacterial activity by Juan Mongolian and others (2016) show that hydrolat has short storage time and its antibacterial activity is not obvious all the time. (2017, the academic workshop of China ornamental horticulture, which discloses the extraction and antibacterial property of 8 garden plant hydrolat in Beijing area and the research of crowd feedback) there is also a process for preparing the hydrolat skin care product by extracting the components of the leaf cyan alcohol, the citronellol and the phenethyl alcohol in the rose hydrolat, but the treatment process is complex and the antioxidant activity is not high.

CN112076106A, a chinese patent discloses a preparation method of skin care lotion of double-petal red rose, wherein the traditional preparation process of the lotion adopts an autoclave method, which can ensure the quality guarantee of the lotion during the extraction and encapsulation processes, but can not prolong the quality guarantee period of the unsealed lotion, and at the same time, does not improve the activity thereof.

Disclosure of Invention

In view of the above, the invention aims to provide a long-acting fresh-keeping skin-care type hydrolat based on natural traditional Chinese medicines and a preparation method thereof. The invention uses plant extracts as natural antistaling agent to promote the fresh-keeping effect of rose hydrosol. The pure dew provided by the application has high tyrosinase removal rate, high DPPH clearance rate and antibacterial activity, can be used as a cosmetic pure dew raw material and a facial mask pure dew moisturizing component to replace a pure dew stock solution, is simple in preparation process, is short in growth period, high in productivity, low in cost, free of adding a chemical preservative, simplified in production process and high in chemical activity, and the components are all derived from plant sources.

The technical scheme provided by the invention is as follows:

a long-acting fresh-keeping hydrolat is prepared from plant-derived hydrolat stock solution and bacteriostatic Chinese medicinal materials; the bacteriostatic traditional Chinese medicinal materials are selected from one or more of folium artemisiae argyi, honeysuckle, pepper, semen cassiae, fennel and litsea cubeba.

The plant source hydrolat stock solution is rose hydrolat stock solution. The stock solution of the rose hydrosol is prepared from fresh rose petals or dried rose petals.

The preparation method of the long-acting fresh-keeping hydrolat comprises the following steps:

s1, grinding the hydrolat plant source raw materials into powder, adding sterile water, carrying out reduced pressure distillation to obtain plant source hydrolat crude extract, and then filtering by adopting a microporous filter membrane to obtain filtrate which is plant source hydrolat stock solution;

s2, mixing the bacteriostatic traditional Chinese medicinal materials with the plant-derived hydrolat stock solution prepared in the step S1, sealing and placing for 7-14 days, filtering, and collecting filtrate to obtain the long-acting fresh-keeping hydrolat.

In step S2, the weight parts of the plant source hydrolat stock solution are 70-90 parts, and the weight parts of the bacteriostatic traditional Chinese medicinal materials are 3-10 parts.

In step S1, the conditions of the reduced pressure distillation are: the rotation speed is 25-30r/min, the pressure is 0.09-0.1mPa, the temperature is 90-100 ℃, and the distillation time is 1-2 hours.

As another embodiment of the invention, the preparation method of the long-acting refreshing pure dew comprises the following steps:

A. grinding the hydrolat plant source raw materials into powder, adding sterile water, placing the powder in a reduced pressure distillation device for reduced pressure distillation to obtain plant source hydrolat crude extract, and filtering to obtain filtrate which is sterile plant source hydrolat stock solution;

B. the antibacterial traditional Chinese medicinal materials are mixed according to the mass ratio of the traditional Chinese medicines to water of 1: 10-20 mixing and leaching, standing and extracting for 1-3 weeks, and filtering to obtain Chinese medicinal leaching liquor;

C. mixing the Chinese medicinal leaching liquor and the plant source pure dew stock solution to obtain the long-acting fresh-keeping pure dew.

In the step C, the mass ratio of the traditional Chinese medicine leaching liquor to the plant source hydrolat stock solution is 1: 9-1:12.

In the step A, the reduced pressure distillation conditions are as follows: the rotation speed is 25-30r/min, the pressure is 0.09-0.1mPa, the temperature is 90-100 ℃, and the distillation time is 1-2 hours.

The hydrolat plant source raw material is fresh rose petals or dried rose petals.

The invention relates to an application of the long-acting fresh-keeping hydrolat in skin care products, belonging to the protection scope of the invention.

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

(1) the rose hydrolat formula with tyrosinase removal rate of 50.70-88.15% and DPPH clearance of 80.60-92.80% is prepared by specifically adding natural traditional Chinese medicines or extracts into the rose hydrolat stock solution and further preferably selecting the types and the addition range of the traditional Chinese medicines.

(2) By adopting the method, the rose hydrosol with high tyrosinase removal rate, high DPPH removal rate and antibacterial activity is prepared, can be used as a cosmetic hydrosol raw material and a mask hydrosol moisturizing component to replace hydrosol stock solution, and is simple in preparation process, short in growth cycle, high in productivity and low in cost, and the components are all from plant sources.

(3) The product prepared by the method has long preservation period, and has the characteristics of no need of adding a chemical preservative, simplified production process and high chemical activity. Compared with the existing pure dew which is not easy to preserve after being uncovered, the shelf life of the formula treatment is greatly prolonged.

Drawings

Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:

FIG. 1 is a schematic diagram of the preparation of long-acting fresh-keeping hydrolat by the direct addition method of the present invention;

FIG. 2 is a schematic diagram of a blending method for preparing long-acting fresh-keeping hydrolat.

Detailed Description

The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention.

The technical scheme provided by the invention is as follows:

a long-acting fresh-keeping hydrolat comprises plant source hydrolat stock solution and bacteriostatic traditional Chinese medicinal materials selected from one or more of folium Artemisiae Argyi, flos Lonicerae, fructus Zanthoxyli, semen Cassiae, fructus Foeniculi and fructus Litseae.

The plant source hydrolat stock solution is rose hydrolat stock solution;

the hydrolat plant source comprises fresh rose petals (Rosa rugosa) and dried rose petal products;

the sterile water is selected from one of deionized water, purified water and distilled water.

EXAMPLE 1 preparation of stock solution of dried Rose Bengal

The preparation method comprises the following steps:

1. taking 50g of dried red rose with multiple petals;

2. grinding the dried flowers into powder;

3. pouring the powder into a 250ml three-neck round-bottom flask through a charging hole;

4. pouring 100ml of sterile water;

5. and opening the reduced pressure distillation device, and respectively setting the rotation speed to be 26r/min, the pressure to be 0.09mPa and the pressure to be 96 ℃ and distilling for 1 hour.

6. And after distillation, filtering the obtained rose hydrosol stock solution by adopting a 0.22-micron microporous filter membrane, filling into a brown bottle, and packaging by using sealing glue to obtain the sterile dry rose hydrosol stock solution.

Example 2 preparation of stock solution of fresh flower rose hydrosol

The preparation method comprises the following steps:

1. taking 100g of fresh red rose with multiple petals;

2. grinding fresh flowers into powder;

4. pouring 100ml of sterile water;

6. And after distillation, filtering the obtained rose hydrosol stock solution by using a 0.22-micron microporous filter membrane, filling into a brown bottle, and packaging by using sealing glue to obtain sterile fresh flower rose hydrosol stock solution.

Examples 3 to 10

The long-acting fresh-keeping hydrolat is prepared by a direct addition method, and is shown in figure 1.

The preparation method comprises the following steps:

1. fully air-drying and sterilizing the surface of the bacteriostatic traditional Chinese medicinal material before directly adding the bacteriostatic traditional Chinese medicinal material, and adding the traditional Chinese medicinal material into brown bottles in a clean workbench according to the table 1 respectively;

2. filtering with 0.22 μm microporous membrane, filling the stock solution of dried flower and flos Rosae Rugosae hydrosol prepared in example 1 or the stock solution of flower and flos Rosae Rugosae hydrosol prepared in example 2 into brown bottle containing bacteriostatic Chinese medicinal materials, and packaging with sealing glue; continuously leaching the effective components of the bacteriostatic traditional Chinese medicinal materials by using a water dispersion system in a brown bottle, standing for 7 days, and filtering to obtain the long-acting fresh-keeping hydrolat.

TABLE 1 (parts by weight)

Examples 11 to 18

The long-acting fresh-keeping hydrosol is prepared by blending method, as shown in FIG. 2.

1. Respectively mixing folium artemisiae argyi (Artemisia argyi), honeysuckle (Lonica japonica), pepper (Zanthoxylum bungeanum), Cassia seed (Cassia toraLinn), common fennel (Foeniculum vulgare) and Litsea cubeba (Litsea cubeba) according to the mass ratio of traditional Chinese medicines to water of 1: 10, mixing and leaching, standing and extracting for 1 week, and filtering to obtain a traditional Chinese medicine leaching liquor;

2. the traditional Chinese medicine water extract is injected into a brown bottle in a clean bench by using a 0.22 mu m microporous filter membrane, the dried flower rose hydrosol stock solution prepared in example 1 or the flower rose hydrosol stock solution prepared in example 2 is injected into the brown bottle by using the 0.22 mu m microporous filter membrane, and the traditional Chinese medicine water extract and the hydrosol stock solution are mixed according to the mass ratio shown in the table 2 to obtain the long-acting fresh-keeping hydrosol prepared by a blending method.

TABLE 2 (parts by weight)

Comparative example 1

The stock solution of the dried rose hydrolat prepared in example 1 was autoclaved under the following conditions: 102.9kPa, the temperature reaches 121 ℃, and the sterilization is carried out for 20 minutes.

Comparative example 2

The stock solution of fresh flower rose hydrosol prepared in example 2 was autoclaved under the following conditions: 102.9kPa, the temperature reaches 121 ℃, and the sterilization is carried out for 20 minutes.

Example 19 effect test 1:

tyrosinase removal rate

This example 19 was conducted to measure the tyrosinase activity inhibition rate in examples 3 to 18 and comparative examples 1 and 2; the tyrosinase activity inhibition rate is determined according to ' Shanghai daily chemical industry Association ' standard ' T/SHRH 015-2018, wherein the higher the tyrosinase activity inhibition rate is, the higher the activity of the hydrolat is.

The results are shown in Table 3, and the results in Table 3 show that:

in the fresh flower hydrolat and the dried flower hydrolat, the tyrosinase inhibition rate of the fresh flower hydrolat is obviously higher than that of the dried flower hydrolat.

Compared with the high-pressure sterilization method in the traditional hydrolat preparation process, the method can prolong the shelf life of the hydrolat after being unsealed and improve the activity of the hydrolat.

TABLE 3 tyrosinase removal rate

Example 20 effect test 2:

DPPH radical scavenging Rate determination

Example 20 DPPH removal was measured for examples 1-19 and comparative examples 1 and 2 and the results are shown in table 4:

test methods reference: determination of antioxidant Activity of 17 plants by DPPH method [ J ] food technology, 2006,000(010):264-268.

Wherein, the higher the DPPH free radical clearance rate is, the better the hydrolat activity is.

TABLE 4DPPH radical scavenging assay

The DPPH radical scavenging test results for each formulation are shown in table 4. The best results after 4 weeks of storage were 92.82%, 95.44%, 92.78% for examples 6, 14, 18, respectively, which were better than comparative example 2 (68.81%) after 4 weeks of storage, and also better than example 1 (68.80%) and example 2 (86.30%).

The test result shows that the activity of the hydrolat directly added group is better maintained after four weeks, the method reduces the treatment process of the traditional Chinese medicinal materials, the water dispersion system continuously leaches the water-soluble components in the traditional Chinese medicinal materials, and the traditional Chinese medicinal materials have higher utilization rate and more lasting effect compared with the mode of carrying out pre-extraction and blending on the traditional Chinese medicinal materials. Taking the addition of the cassia seeds as an example, the traditional Chinese medicine of the cassia seeds is rich in anthraquinone compounds such as emodin, obtusin and physcion, has higher antibacterial activity compared with flavonoid substances in the rose hydrosol, and is cooperated with active ingredients such as citronellol, linalool and terpineol in the hydrosol solution, so that the oxidation resistance characteristics such as tyrosinase activity removal rate, DPPH removal rate and the like are improved.

Example 21 effect test 3:

bacteriostasis test

In this example, the hydroluses prepared in examples 3 to 18 and comparative examples 1 and 2 were tested in the bacteriostasis test.

The specific steps of the supplementary bacteriostasis test are as follows:

1. sampling, soaking cotton swabs with 0.9% physiological saline, sampling at five points, and selecting Escherichia coli as a test strain.

2. NA medium plates were prepared. The formula is as follows: preparing 1L of 33g of culture medium, preparing 200ml of culture medium, and metering the volume of 6.6gNA culture medium in each bottle to 200 ml;

3. autoclaving, and pouring into a flat plate;

4. placing the antibacterial liquid to be detected in a conical flask, cutting a filter paper wafer with the diameter of 0.6cm, soaking in the antibacterial liquid to be detected for 1 week, taking out, and air-drying for later use;

5. inoculating Escherichia coli slant strain in culture medium by coating method, placing into filter paper carrying antibacterial solution, and measuring its antibacterial diameter after 48 hr to obtain antibacterial effect measurement index.

The results are shown in Table 5:

TABLE 5 zone of inhibition diameter

The results in table 5 show that, in the results of the common bacteriostatic ability test of the direct addition method and the blending method, the most obvious bacteriostatic effect is the hydrolat + cassia seed, the diameter of the bacteriostatic circle reaches 1.9cm after the plant is placed for 4 weeks, and the bacteriostatic effect difference of other groups is not obvious compared with that of the pure hydrolat of fresh flower rose. The cassia seed has the most remarkable bacteriostatic ability after 4 weeks.

In the research, compared with the blending group, the activity of the hydrolat directly added group is better maintained after four weeks, but in the result of the bacteriostatic test, the fresh flower hydrolat and the cassia seed show stronger microbial inhibition effect, and the diameter of the bacteriostatic zone reaches 1.9cm, which is more than 30% of that of the pepper and fennel added group. Meanwhile, in the actual addition, the pepper and the fennel have heavier own tastes, the taste quality of the rose hydrosol is slightly influenced, and the cassia seed has no own taste. Comprehensively considered, the best combination for promoting the fresh-keeping and skin-care effects of the fresh flower rose hydrosol is the fresh flower rose hydrosol and the cassia seed (direct addition method).

The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.

Claims

1. The long-acting fresh-keeping hydrolat is characterized by comprising plant source hydrolat stock solution and bacteriostatic traditional Chinese medicinal materials; the bacteriostatic traditional Chinese medicinal materials are selected from one or more of folium artemisiae argyi, honeysuckle, pepper, semen cassiae, fennel and litsea cubeba.

2. The long-acting refreshing hydrolat as claimed in claim 1, wherein the plant-derived hydrolat stock solution is rose hydrolat stock solution.

3. The method for preparing the long-acting refreshing pure dew as claimed in claim 1, which comprises the following steps:

s1, grinding the hydrolat plant source raw materials into powder, adding sterile water, carrying out reduced pressure distillation to obtain plant source hydrolat crude extract, and filtering to obtain filtrate as plant source hydrolat stock solution;

4. The method according to claim 3, wherein in step S1, the hydrolat-derived material is fresh rose petals or dried rose petals.

5. The preparation method according to claim 3, wherein in step S2, the weight portion of the plant-derived hydrolat stock solution is 70-90 parts, and the weight portion of the bacteriostatic traditional Chinese medicinal material is 3-10 parts.

6. The production method according to claim 3, wherein in step S1, the conditions of the reduced pressure distillation are as follows: the rotation speed is 25-30r/min, the pressure is 0.09-0.1mPa, the temperature is 90-100 ℃, and the distillation time is 1-2 hours.

7. The method for preparing the long-acting refreshing pure dew as claimed in claim 1, which comprises the following steps:

A. grinding the hydrolat plant source raw materials into powder, adding sterile water, carrying out reduced pressure distillation to obtain plant source hydrolat crude extract, and filtering to obtain filtrate which is sterile plant source hydrolat stock solution;

8. The preparation method according to claim 7, wherein in the step C, the mass ratio of the traditional Chinese medicine leaching liquor to the plant-derived hydrolat stock solution is 1:9-1: 12.

9. The process according to claim 7, wherein in the step A, the reduced pressure distillation conditions are as follows: the rotation speed is 25-30r/min, the pressure is 0.09-0.1mPa, the temperature is 90-100 ℃, and the distillation time is 1-2 hours.

10. Use of the long-lasting preservative syrup according to claim 1 or 2 in a skin care product.