CN112156049A

CN112156049A - Plant hydrolat and preparation method thereof

Info

Publication number: CN112156049A
Application number: CN202011244545.9A
Authority: CN
Inventors: 朱虹; 石锋; 李灵卫; 岑梦珍; 吴文; 饶梦晴; 史晋轩
Original assignee: Zhejiang Qianqianning Biotechnology Co Ltd
Current assignee: Zhejiang Qianqianning Biotechnology Co Ltd
Priority date: 2020-11-10
Filing date: 2020-11-10
Publication date: 2021-01-01

Abstract

The invention discloses a plant hydrolat and a preparation method thereof, which comprises the following steps; s1 processing the raw material; s2 steam distillation; s3 collecting the condensate; s4, oil-water separation; s5 ultrafiltration crude product hydrolat; s6, sterilizing; s7 mixing; and S8, filling and leaving factory. The plant hydrolat prepared by the invention has higher essential oil content, has better moisturizing effect on skin after being used, and can play a role in improving skin occlusion, shrinking pores and improving skin fineness.

Description

Plant hydrolat and preparation method thereof

Technical Field

The invention relates to the field of cosmetics, and in particular relates to plant hydrolat and a preparation method thereof.

Background

The verbenam Rosemary is a famous and precious natural spice plant with long history in the original European regions of Rosemary and the coastal coast of the northern part of Africa, is named as Rosemary Verbenone in English and named as Korean in the sea, and is a well-known plant with high antioxidation. The plants are upright, the leaves are narrow and sharp, the shape of the plants is similar to that of bent pine needles, the leaf edges curl to the leaf backs, the flowers are blue, and the plants grow in small clusters in the axils of the leaves. The research shows that it has good application prospect in the fields of cosmetics, foods, medicines and the like.

Researches show that the verbenam and rosemary contain chemical components such as monoterpenes and ketones, have strong contraction effect, can tighten loose skin, can relieve the congestion and swelling of the skin, and has good curative effect on acne, particularly closed-mouth acne. The hydrolat extracted from the flowers and twigs of the plant essential oil contains natural and pure components and light and pleasant fragrance, contains plant essential oil components, is easy to be absorbed by skin, is mild and non-irritant, can be frequently used, and has good market expansibility.

At present, the method for preparing plant hydrolat and essential oil at home and abroad is mainly a distillation method, namely, the essential oil in plant tissues is separated and extracted by using the evaporation characteristic of the essential oil at high temperature and using steam as a transmission medium. However, in the preparation process, the materials are kept at high temperature for a long time, and the main components of the materials have the hidden trouble of decomposition, so that the problem that the prepared plant hydrolat is low in quality can be caused; however, the extraction preparation is carried out at a relatively low temperature, and the problem of low content of essential oil in the plant hydrolat exists. The extraction auxiliary agent is added in the process of preparing the plant hydrolat, so that the content of the essential oil can be effectively improved; therefore, how to improve the content and quality of the essential oil in the hydrolat by modifying and optimizing the extraction auxiliary agent has important significance.

Disclosure of Invention

The hydrolat is a 100% saturated distillation stock solution separated during the extraction of essential oil during the distillation extraction process, and the components are natural and pure. The content of the essential oil in the hydrolat is a main index for identifying the quality of the hydrolat, and the higher the content of the essential oil, the more precious the hydrolat is, and the better the quality of the hydrolat is. Because most of the chemical components of the essential oil are fat-soluble and insoluble in water, there is no effective method in the industry how to increase the content of the essential oil in the hydrolat.

The invention aims to provide the plant hydrolat which has higher essential oil content, has better moisturizing effect on skin after being used, and can play roles in improving skin occlusion, shrinking pores and improving skin fineness.

The second purpose of the invention is to provide a preparation method of the plant hydrolat.

In order to achieve the purpose, the invention adopts the technical scheme that:

a preparation method of plant hydrolat comprises the following steps:

s1 processing raw materials: selecting uniform and non-rotten verbena-meyeriana leaves, and removing impurities;

s2 steam distillation: sequentially adding 10-20 kg of water, 0.1-0.2 kg of enzyme, 0.1-0.2 kg of surfactant, 1-2 kg of extraction aid and 100-200 kg of verbena officinalis leaf into a distillation device, uniformly stirring, carrying out enzymolysis at 40-60 ℃ for 1-3h, then distilling, setting the steam amount to be 40-60L/h, the vacuum degree to be 8.00-20.00 kPa, the temperature to be 40-50 ℃, and distilling for 2-4 h;

s3 collecting the condensate: condensing the mixed gas of the pure dew and the steam generated by distillation, wherein the temperature of the condensation is set to be 10-20 ℃, and collecting distillate;

s4 oil-water separation: separating oil and water from the distillate, and separating the lower layer hydrolat from the upper layer essential oil to obtain crude hydrolat;

s5 ultrafiltration crude hydrolat: performing ultrafiltration on the crude hydrolat to obtain refined hydrolat;

s6 sterilization: performing heat sterilization treatment on the refined hydrolat;

s7 mixing: adding antiseptic into the sterilized refined hydrolat, and stirring;

s8, filling and leaving factory: and (4) filling in a sterile environment to obtain the plant hydrolat. Preferably, the plant is verbena officinalis.

The material of the extraction device in the distillation device is any one of iron, copper, aluminum and stainless steel, and preferably, the material of the extraction device in the distillation device is copper.

The enzyme is one or more than two of cellulase, neutral protease, alpha-amylase and pectinase. Preferably, the enzyme is prepared from cellulase and pectinase according to the mass ratio of (1-2): 1.

The surfactant is one or a mixture of two or more of disodium lauryl sulfosuccinate, disodium cocomonoethanolamide sulfosuccinate, lauramidopropyl hydroxysultaine and lauramidopropyl amine oxide. Preferably, the surfactant is disodium cocomonoethanolamide sulfosuccinate.

The preservative is one of chlorobutanol, climbazole, bis (hydroxymethyl) imidazolidinyl urea and p-hydroxyacetophenone. The addition amount of the preservative is 0.05-0.1% of the mass of the refined hydrosol.

The extraction auxiliary agent is at least one of alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin, hydroxypropyl-beta-cyclodextrin and modified beta-cyclodextrin. Preferably, in some embodiments of the present invention the extraction aid is hydroxypropyl- β -cyclodextrin.

Further preferred, in some embodiments of the invention the extraction aid is a modified beta-cyclodextrin; preferably, the preparation method of the modified beta-cyclodextrin comprises the following steps: adding 1-5 parts by weight of beta-cyclodextrin into 5-10 parts by weight of 20-35 wt% sodium hydroxide solution, and stirring for 5-15 h; then adding 1-3 parts by weight of epoxy chloropropane, and reacting for 1-3h at 25-35 ℃; after the reaction is finished, adding 40-50 parts by weight of acetone, standing for 0.1-2h, and filtering to obtain filter residue; continuously washing the filter residue with acetone, adding the filter residue into 35-50 parts by weight of water, stirring uniformly, adjusting the pH value to be neutral, and standing for 30-50 h; then adding 150 plus 200 weight parts of absolute ethyl alcohol, standing for 0.5-2h, filtering and drying to obtain the product.

Further preferably, the preparation method of the modified beta-cyclodextrin comprises the following steps: adding 1-5 parts by weight of beta-cyclodextrin into 5-10 parts by weight of 20-35 wt% sodium hydroxide solution, and stirring for 5-15 h; then adding 1-3 parts by weight of epoxy chloropropane, and reacting for 1-3h at 25-35 ℃; after the reaction is finished, adding 40-50 parts by weight of acetone, standing for 0.1-2h, and filtering to obtain filter residue; continuously washing the filter residue with acetone, adding the filter residue into 35-50 parts by weight of water, stirring uniformly, adjusting the pH value to 4.5-5.5, adding 0.01-0.1 part by weight of pullulanase, reacting at 60-70 ℃ for 35-50h, and adjusting the pH value to be neutral after the reaction is finished; then adding 150 plus 200 weight parts of absolute ethyl alcohol, standing for 0.5-2h, filtering and drying to obtain the product.

The pure copper distillation device adopted by the invention is soft and tough in texture, rich in ductility, even in heating, capable of keeping the temperature stable for a long time, higher in density than stainless steel and 10 times as high in heat conduction as a stainless steel pot, so that the penetrability and the function of force fragrance are strong, all essences in the verbena officinalis can be extracted more completely, and the content of essential oil in the hydrolat is effectively increased.

The invention adds specific enzyme in the extraction process, plays a role in destroying the cell structure of the verbena, the rosemary and the verbena, enables the extracted substance to be released from the cells more easily and extracted, and has the advantages of high efficiency, simple and convenient operation, mild conditions and the like. Furthermore, a certain amount of surfactant is added in the enzymolysis process, so that the enzymolysis reaction can be effectively promoted. Surfactant-assisted enzymatic hydrolysis may facilitate enzymatic hydrolysis by affecting the processes of adsorption and desorption of the enzyme from the substrate, reducing the efficiency of enzyme adsorption and thus enzyme inactivation. The extraction rate of the essential oil is improved, and the content of the essential oil in the hydrolat is further improved.

In order to improve the content of the essential oil in the hydrolat, the extraction aid cyclodextrin is added in the distillation extraction process, and the cyclodextrin is cyclic oligosaccharide and generally contains 6-12D-glucopyranose units. Common are alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin, which are respectively formed by connecting 6, 7 and 8 glucopyranose units by alpha- (1, 4) -glycosidic bonds. Because the water soluble polymer has an internal hydrophobic and external hydrophilic annular space structure in an aqueous solution, the water soluble polymer can form an inclusion compound with fat soluble molecules with proper size, and further improves the water solubility, bioavailability and stability of fat soluble components. According to the invention, by utilizing the internal hydrophobic and external hydrophilic annular space structure of cyclodextrin, the fat-soluble molecules of essential oil enter the cyclodextrin cavity to form an inclusion compound in the distillation and extraction process, and the content of the essential oil in the hydrolat is greatly improved in a large amount of dissolved aqueous solution.

Although cyclodextrin, especially beta-cyclodextrin, has the advantages of low price, moderate cavity and the like, the cyclodextrin has low water solubility. The invention artificially improves the content of essential oil in the hydrolat, and adopts hydroxypropyl-beta-cyclodextrin as an extraction auxiliary agent; as the hydroxypropyl derivative of the beta-cyclodextrin, the hydroxypropyl has better water solubility because the introduction of the hydroxypropyl destroys the hydrogen bonds in the molecule; furthermore, the invention adopts modified beta-cyclodextrin as an extraction auxiliary agent; compared with unmodified beta-cyclodextrin, the modified beta-cyclodextrin has an epoxy group and/or glycosyl active structure in the outer surface, has higher water solubility, and further improves the content of volatile components in the hydrolat.

Detailed Description

In the examples, the sources of the raw materials are as follows:

verbena officinalis leaf: hunan of origin

A distillation device: comprises an extraction device, a condenser, an oil-water separator and a vacuum pump.

Cellulase: : the enzyme activity is 1 wu/g, and the enzyme activity is purchased from Nanning Dong Henghuadao biological technology, Inc.

And (3) pectinase: the enzyme activity is 1-3 wu/g, and is purchased from Nanning Dong Henghuadao biological technology, Inc.

Disodium cocomonoethanolamide sulfosuccinate: CAS number; 61791-66-0, purchased from Wuhan Yuancheng science and technology Limited.

Disodium lauryl sulfosuccinate monoester: CAS number; 19040-44-9, available from Sendzein, Shenzhen, Sendzi Biotech, Inc.

Lauramidopropyl amine oxide: CAS number; 61792-31-2, available from Hebei Hengjing chemical Co., Ltd.

Lauramidopropyl hydroxysultaine: purchased from biosciences, church, su.

Alpha-cyclodextrin; beta-cyclodextrin; gamma-cyclodextrin; hydroxypropyl-beta-cyclodextrin; CAS number; 128446-35-5, all available from Zhiyuan Biotech, Inc., Binzhou, Shandong.

P-hydroxyacetophenone: CAS: 99-93-4, purchased from Wuhanxing Zhongcheng science and technology Limited.

Example 1

A preparation method of plant hydrolat comprises the following steps:

s2 steam distillation: sequentially adding 150kg of verbena officinalis leaves into a distillation device, setting the steam amount to be 50L/h, the vacuum degree to be 10.00kPa, the temperature to be 45 ℃, and distilling for 3 h;

s3 collecting the condensate: condensing the mixed gas of the pure dew and the steam generated by distillation, opening a condenser, and connecting cooling water; controlling the temperature of effluent liquid cooled by the condenser to be 20 ℃ by using cooling water within half an hour after boiling; after half an hour, the temperature of the effluent liquid is raised to 30 ℃ and kept stable until the end; and collecting the distillate;

s4 oil-water separation: separating oil and water from the distillate, refluxing the distillate into the distillation device after separation by the oil-water separator for 3 hours, closing the reflux valve, opening the collection valve, and collecting the water layer to obtain crude distillate;

s5 ultrafiltration crude hydrolat: performing ultrafiltration on the crude hydrolat to obtain refined hydrolat; the aperture of the ultrafiltration membrane is 10 μm, the operating pressure is 0.4MPa (2-4 kg/cm), and the permeation rate of the membrane is 3 m/(m.d).

S6 sterilization: sterilizing the refined hydrolat at 100 deg.C for 5 min;

s7 mixing: adding p-hydroxyacetophenone into the sterilized refined hydrolat, and stirring uniformly; the adding amount of the p-hydroxyacetophenone is 0.1 percent of the mass of the refined pure dew;

s8, filling and leaving factory: and (4) filling in a sterile environment to obtain the plant hydrolat.

The extraction device in the distillation device is made of copper.

Example 2

Essentially the same as example 1, the only difference being:

the material of an extraction device in the distillation device is iron.

Example 3

Essentially the same as example 1, the only difference being:

the material of an extraction device in the distillation device is aluminum.

Example 4

Essentially the same as example 1, the only difference being:

the material of an extraction device in the distillation device is stainless steel.

Example 5

A preparation method of plant hydrolat comprises the following steps:

s2 steam distillation: sequentially adding 15kg of water, 0.15kg of enzyme, 0.15kg of surfactant, 1.5kg of extraction aid and 150kg of verbena officinalis leaf into a distillation device, uniformly stirring, carrying out enzymolysis at 45 ℃ for 2h, then distilling, setting the steam amount to be 50L/h, the vacuum degree to be 10.00kPa, the temperature to be 45 ℃, and distilling for 3 h;

S6 sterilization: sterilizing the refined hydrolat at 100 deg.C for 5 min;

The material of an extraction device in the distillation device is copper.

The enzyme is cellulase and pectinase according to the mass ratio of 1: 1 are mixed.

The surfactant is disodium cocomonoethanolamide sulfosuccinate monoester.

The extraction auxiliary agent is hydroxypropyl-beta-cyclodextrin.

Example 6

Essentially the same as example 5, the only difference being:

the enzyme is cellulase.

Example 7

Essentially the same as example 5, the only difference being:

the enzyme is pectinase.

Example 8

Essentially the same as example 5, the only difference being:

the surfactant is disodium lauryl sulfosuccinate monoester.

Example 9

Essentially the same as example 5, the only difference being:

the surfactant is lauramidopropyl hydroxysulfobetaine.

Example 10

Essentially the same as example 5, the only difference being:

the surfactant is lauramidopropyl amine oxide.

Example 11

Essentially the same as example 5, the only difference being:

the extraction auxiliary agent is alpha-cyclodextrin.

Example 12

Essentially the same as example 5, the only difference being:

the extraction auxiliary agent is beta-cyclodextrin.

Example 13

Essentially the same as example 5, the only difference being:

the extraction auxiliary agent is gamma-cyclodextrin.

Example 14

Essentially the same as example 5, the only difference being:

the extraction auxiliary agent is modified beta-cyclodextrin; the preparation method of the modified beta-cyclodextrin comprises the following steps: adding 3 parts by weight of beta-cyclodextrin into 7 parts by weight of 30 wt% sodium hydroxide solution, and stirring for 10 hours; then adding 1.8 parts by weight of epoxy chloropropane, and reacting for 1.8h at 32 ℃; after the reaction is finished, adding 45 parts by weight of acetone, standing for 0.5h, and filtering to obtain filter residue; continuously washing the filter residue with acetone for 2 times, adding the filter residue into 36 parts by weight of water, uniformly stirring, adjusting the pH value to be neutral, and standing for 36 hours; adding 180 parts by weight of absolute ethyl alcohol, standing for 1 hour, filtering and drying to obtain the product. The epichlorohydrin, CAS: 106 to 89 to 8 percent and the purity of 99.6 percent, and is purchased from chemical industry Co., Ltd of Hua Wei Rui, Beijing.

Example 15

Essentially the same as example 5, the only difference being:

the extraction auxiliary agent is modified beta-cyclodextrin; the preparation method of the modified beta-cyclodextrin comprises the following steps: adding 3 parts by weight of beta-cyclodextrin into 7 parts by weight of 30 wt% sodium hydroxide solution, and stirring for 10 hours; then adding 1.8 parts by weight of epoxy chloropropane, and reacting for 1.8h at 32 ℃; after the reaction is finished, adding 45 parts by weight of acetone, standing for 0.5h, and filtering to obtain filter residue; continuously washing the filter residue with acetone for 2 times, adding the filter residue into 36 parts by weight of water, uniformly stirring, adjusting the pH value to 5.0, adding 0.06 part by weight of pullulanase, reacting at 62 ℃ for 36 hours, and adjusting the pH value to be neutral after the reaction is finished; adding 180 parts by weight of absolute ethyl alcohol, standing for 1 hour, filtering and drying to obtain the product. The pullulanase has the following advantages: the enzyme activity is 1000u/g, and the enzyme activity is purchased from Shanghai Kanglang biological technology limited. The epichlorohydrin, CAS: 106 to 89 to 8 percent and the purity of 99.6 percent, and is purchased from chemical industry Co., Ltd of Hua Wei Rui, Beijing.

Comparative example 1

A preparation method of plant hydrolat comprises the following steps:

s2 steam distillation: sequentially adding 15kg of water, 0.15kg of surfactant, 1.5kg of extraction aid and 150kg of verbena and rosemary leaves into a distillation device, uniformly stirring, carrying out enzymolysis at 45 ℃ for 2h, then distilling, setting the steam amount to be 50L/h, the vacuum degree to be 10.00kPa, the temperature to be 45 ℃, and distilling for 3 h;

S6 sterilization: sterilizing the refined hydrolat at 100 deg.C for 5 min;

The extraction device in the distillation device is made of copper.

The surfactant is disodium cocomonoethanolamide sulfosuccinate monoester.

The extraction auxiliary agent is hydroxypropyl-beta-cyclodextrin.

Comparative example 2

A preparation method of plant hydrolat comprises the following steps:

s2 steam distillation: sequentially adding 15kg of water, 0.15kg of enzyme, 1.5kg of extraction aid and 150kg of verbena and oxadiazon rosemary leaves into a distillation device, uniformly stirring, carrying out enzymolysis for 2h at 45 ℃, distilling, setting the steam amount to be 50L/h, the vacuum degree to be 10.00kPa, the temperature to be 45 ℃, and distilling for 3 h;

S6 sterilization: sterilizing the refined hydrolat at 100 deg.C for 5 min;

The extraction device in the distillation device is made of copper.

The extraction auxiliary agent is hydroxypropyl-beta-cyclodextrin.

Comparative example 3

A preparation method of plant hydrolat comprises the following steps:

s2 steam distillation: sequentially adding 15kg of water, 0.15kg of enzyme, 0.15kg of surfactant and 150kg of verbena and oxadiazon rosemary leaves into a distillation device, uniformly stirring, carrying out enzymolysis for 2h at 45 ℃, distilling, setting the steam amount to be 50L/h, the vacuum degree to be 10.00kPa, the temperature to be 45 ℃, and distilling for 3 h;

S6 sterilization: sterilizing the refined hydrolat at 100 deg.C for 5 min;

The extraction device in the distillation device is made of copper.

The surfactant is disodium cocomonoethanolamide sulfosuccinate monoester.

Test example 1:

and (3) measuring the content of volatile components in the hydrolat:

the essential oil in the plant hydrosol mainly contains monoterpene, sesquiterpene, alcohols, esters, ketones, oxides and other volatile components.

The test method comprises the following steps: refer to patent CN 105929099A, a method for detecting volatile components in hydrolat, the test method disclosed in example 1 in the specification.

The specific test method is as follows:

the sample is the verbena rosemary hydrolat prepared in each example and comparative example.

1. Sample pretreatment:

(1) sample weighing: sample 2g (to the nearest 0.0001g) was accurately weighed in a 20mL headspace bottle using an analytical balance.

(2) Addition of saturated sodium chloride solution: accurately 1.0mL of saturated sodium chloride solution was added to the headspace bottle.

(3) Adding an internal standard substance: a0.1 mL solution of 2-hexanone (0.05mg/mL) was added to the headspace.

2. Head space conditions

The constant temperature is 90 ℃; the temperature of the sampling needle is 110 ℃; the temperature of a transmission line is 130 ℃, and the balance time of a headspace sample injection sample is 60 min; pressurizing the sample bottle for 1.5 min; sample introduction time is 0.15 min; needle pulling time is 0.2 min; the sample inlet pressure is higher than the highest chromatographic pressure of 35 Psi.

3. Chromatographic conditions

HP-5MS capillary column (60m × 0.25mm × 0.25 μm) is adopted; the temperature of a sample inlet is 250 ℃; column oven temperature program: the initial temperature is 60 ℃, the temperature is raised to 170 ℃ at the speed of 2 ℃/min, and then the temperature is raised to 250 ℃ at the speed of 50 ℃/min and kept for 5.4 min; carrier gas: high purity helium gas; the carrier gas flow is 1.0 mL/min; the split ratio is 10: 1; and the split gas enters mass spectrum detection after being separated by gas chromatography.

4. Conditions of Mass Spectrometry

Transmission line temperature 200 ℃, ion source temperature 200 ℃, solvent delay: 1.5 min; the detection mode is a full scan mode (MS-scan).

5. Data processing

NIST library retrieval of a target peak is carried out by adopting a full-scanning atlas to carry out qualitative analysis, and an internal standard method is adopted to carry out quantitative analysis, so that volatile main components and the content thereof in the hydrolat are obtained, and are shown in Table 1.

Table 1: verbena officinalis and rosemary hydrolat detection result

By comparing examples 1 to 4, the volatile component content in the hydrolat is significantly higher than in examples 2 to 4, in example 1, the extraction device of pure copper is adopted. The reason for this is that copper is soft and tough, is rich in ductility, is heated evenly, can keep temperature stable for a long time, has higher density than stainless steel, and has heat conduction 10 times of a stainless steel pot, so the penetrability and the function of forcing incense are strong, can extract all essences in the verbena officinalis more completely, and effectively improves the content of volatile components in the hydrolat.

By comparing examples 5-7 with comparative example 1, specific enzyme is added in the extraction process of examples 5-7, so that the cell structure of the verbenam and rosemary is damaged, the extracted substance is released from the cells more easily and is extracted, and the extraction rate of volatile components is improved. In further embodiment 5, cellulase and pectinase are compounded to realize synergistic interaction, so that the enzymolysis efficiency is further improved, the extraction rate of volatile components is improved, and the content of the volatile components in the hydrolat is further improved.

By comparing examples 5, 8-10 and comparative example 2, in examples 5, 8-10, a certain amount of surfactant is added in the enzymolysis process to effectively promote the enzymolysis reaction, and the surfactant-assisted enzymolysis can promote the hydrolysis of the enzyme by influencing the adsorption and desorption processes of the enzyme from the substrate, so that the adsorption efficiency of the enzyme is reduced, and the inactivation of the enzyme is reduced. The extraction rate of volatile components is improved, and the content of the volatile components in the hydrolat is further improved.

In order to improve the content of volatile components in the hydrolat, the inventor adds extraction auxiliary agent cyclodextrin or modified cyclodextrin in the distillation extraction process in examples 5 and 11 to 15, and utilizes a hydrophobic and hydrophilic annular space structure inside the cyclodextrin, so that volatile component fat-soluble molecules enter a cyclodextrin cavity to form an inclusion compound in the distillation extraction process, and the content of the volatile components in the hydrolat is greatly improved in a large amount of dissolved aqueous solution. In order to further improve the content of volatile components in the hydrolat, the inventors of the present invention adopted modified beta-cyclodextrin as an extraction aid in examples 14 and 15; compared with unmodified beta-cyclodextrin, the modified beta-cyclodextrin has an epoxy group and/or glycosyl active structure in the outer surface, has higher water solubility, and further improves the content of volatile components in the hydrolat.

Test example 2

Test of moisturizing effect of plant hydrolat

The moisturizing effects of the plant hydrolat of examples 1 and 5 and comparative examples 1 to 3 were evaluated with reference to QB/T4256-. The testing instrument adopts a skin moisture tester with model number RY0-1 provided by western chemical instruments (Beijing) science and technology limited.

And (3) testing environmental conditions: 20-22 ℃ and 40-60% of humidity.

Subjects aged 40-60 years, male and female halves, were selected and randomized into 6 groups of 30 individuals each. The subject has skin aging phenomena such as wrinkles, loose skin or dry skin. The subjects were free of serious systemic disease, no active allergic disease, and had not been tested for skin treatment, cosmetic, and other possible effects. The test sites of the subjects were not able to use any cosmetic or topical drug 2 days prior to testing. The subjects had no significant difference in sex, age, disease condition, etc. (P >0.05), and were comparable.

Circular test areas with a diameter of 25mm were marked at uniform cheek marks 5 on both sides of the subject, 100 μ L of the lotion was applied to each test area, and the lotion was uniformly applied to the test areas using a latex finger cot.

After adjusting the apparatus according to the instructions of the skin analysis tester, the measurement of the test area was performed by measuring the initial value of the test area (before using plant hydrolat) and then measuring the moisture content of the skin in the test area 1 hour after using plant hydrolat. Each test area was run in 3 replicates and the test results were averaged.

The skin moisture content increase rate was calculated according to the following formula: phi is (MMvo-MMVt)/MMvo 100%, wherein phi is the skin moisture growth rate; MMvo is the moisture content of the skin prior to application; MMVt is the moisture content of the skin after 1 hour of application.

Table 2: moisturizing effect test result table

Test example 3

Evaluation of product Effect

Firstly, testing a test article: examples 1 and 5 the plant hydrolat prepared

II, the tested people group: 50 women aged between 20 and 50 years

Thirdly, a testing method:

after cleaning the skin at night every day, a proper amount of test article was gently tapped on the face for 28 days, and changes of the face skin were recorded.

According to the evaluation of the testers on the comfort degree of the skin application and the improvement of the skin after use, the evaluation is carried out at room temperature, the good evaluation is recorded, and the average value is taken. The evaluation criteria are as follows:

regarding comfort (50 points): the plant hydrolat does not irritate the skin, the penetration is fast, and the skin is well relaxed; feeling that plant hydrolat is somewhat irritating to the skin is not good;

improvement effect on skin (50 points): after the plant hydrolat is used, the skin occlusion is obviously improved, pores are shrunk, and the skin becomes fine; the whole skin is not good after the plant hydrolat is used;

table 3: evaluation of product Effect

	Example 1	Example 5
			Comfort level (50 minutes)	45	48
Skin improvement effect (50 minutes)	45	49
			Composite score (total score 100 points)	90	97

As can be seen from the above table, after cleaning the skin at night every day, a proper amount of plant hydrolat is taken and lightly tapped on the face for 28 days of continuous use, the hydrolat is mild and not irritant, and the skin of the face is obviously improved.

The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.

Claims

1. The preparation method of the plant hydrolat is characterized by comprising the following steps:

2. The method for preparing plant hydrolat according to claim 1, wherein the extraction aid is at least one of alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin, hydroxypropyl-beta-cyclodextrin, and modified beta-cyclodextrin.

3. The method for preparing plant hydrolat according to claim 2, wherein the modified β -cyclodextrin is prepared by the following steps: adding 1-5 parts by weight of beta-cyclodextrin into 5-10 parts by weight of 20-35 wt% sodium hydroxide solution, and stirring for 5-15 h; then adding 1-3 parts by weight of epoxy chloropropane, and reacting for 1-3h at 25-35 ℃; after the reaction is finished, adding 40-50 parts by weight of acetone, standing for 0.1-2h, and filtering to obtain filter residue; continuously washing the filter residue with acetone, adding the filter residue into 35-50 parts by weight of water, stirring uniformly, adjusting the pH value to be neutral, and standing for 30-50 h; then adding 150 plus 200 weight parts of absolute ethyl alcohol, standing for 0.5-2h, filtering and drying to obtain the product.

4. The method according to claim 1, wherein the material of the extraction device of the distillation device is copper.

5. The method for preparing plant hydrolat according to claim 1, wherein the preservative is one of chlorobutanol, climbazole, bis (hydroxymethyl) imidazolidinyl urea, and p-hydroxyacetophenone.

6. A plant hydrolat prepared by the method of any one of claims 1 to 5.