CN115429740A

CN115429740A - Preparation method and application of micro-molecular plant cell sap

Info

Publication number: CN115429740A
Application number: CN202210994782.XA
Authority: CN
Inventors: 刘胜茂; 肖钰澄; 唐天鹏; 郭春宝; 赵春花; 杨金凤
Original assignee: Yunnan Zhiyuan Biotechnology Co ltd; Kunming Kangerxun Biological Engineering Co ltd
Current assignee: Yunnan Zhiyuan Biotechnology Co ltd; Kunming Kangerxun Biological Engineering Co ltd
Priority date: 2022-08-18
Filing date: 2022-08-18
Publication date: 2022-12-06

Abstract

A preparation method of micro-molecular plant cell sap and application thereof belong to the technical field of plant cosmetics. Soaking and extracting the plant with micro molecular group water at normal temperature and normal pressure, filtering, adsorbing by a macroporous adsorption resin column, freezing a separation solution to the temperature of-25 to-5 ℃, vacuum-pumping at the temperature of 10 to 40 ℃, condensing gaseous substances at low temperature, filtering a condensate by a2 to 5 mu m filter, and sterilizing at ultrahigh pressure and room temperature to obtain the micro molecular plant cell sap. The application is that the obtained micro-molecular plant cell sap can be used as a whole or partial substitute of water in the preparation of cosmetics. The obtained cell sap has higher effective components and heat sensitive components than common plant pure dew cell sap, and has improved skin penetration effect, absorption rate and moisturizing effect. The production does not use steam, and the use of fuel can be reduced. The obtained product is micro-molecular cell sap, has light color, contains most of effective components of volatile small molecular compounds, and can be widely applied in cosmetics, foods, etc.

Description

Preparation method and application of micro-molecular plant cell sap

Technical Field

The invention belongs to the technical field of plant cosmetics, and particularly relates to a preparation method and application of micro-molecular plant cell sap.

Background

At present, the market of cosmetics in the world tends to add pure natural raw materials, and the cosmetics prepared by plant extracts are also called biological cosmetics. The biological cosmetic has good effects of moisturizing, whitening, relieving, acne removing, anti-aging, aroma enhancing and the like, has no irritation to a human body and no toxic or side effect, and is popular in the market.

Patent application No. CN200710007684.8 applies a method for extracting plant cell sap by freezing, after the plant is crushed, the plant needs to be treated at high temperature of 60-100 ℃, and the heat-sensitive active ingredients in the plant cell sap can be inactivated.

Patent application No. CN202111484503.7 applies a plant cell sap extraction method and device, wherein in the preparation process of the method, high temperature of 120-190 ℃ is required to be used for vaporizing cell sap, and thermosensitive active ingredients can also be inactivated.

Similarly, patent application No. CN202010082619.7 is a process and apparatus for extracting leaf plant cell sap, and CN202010082630.3 is a process and apparatus for extracting root plant cell sap, which also use high temperature to extract, resulting in the inactivation of heat-sensitive active ingredients.

The inactivation of the thermosensitive active ingredients can cause poor skin permeability and moisturizing effect of the plant cosmetics prepared from the plant cell sap.

Disclosure of Invention

The invention aims to provide a preparation method of micro-molecular plant cell sap and application thereof aiming at the defects of the prior art, the obtained plant cell sap is micro-molecular cell sap, the effective components of the plant cell sap are superior to those of the prior art, and the plant cell sap is used for preparing plant cosmetics, and the skin permeability and the moisturizing effect of the plant cosmetics are better than those of the existing plant cosmetics.

The preparation method of the micro-molecular plant cell sap comprises the following steps:

1. taking one or more of fresh flowers, stems, leaves and root blocks of plants, adding 3-6 parts of micro molecular group water according to the weight ratio, and soaking and extracting for 4-6 hours at normal temperature and normal pressure;

2. filtering by using a 100-200 mesh screen to obtain a coarse extraction solution;

3. introducing the crude extraction liquid obtained in the step 2 into a macroporous adsorption resin column for adsorption, performing desorption separation by using micromolecular water with the volume of 3-5 columns, and collecting effluent liquid to obtain a macroporous adsorption separation liquid, wherein the macroporous resin is one or a mixture of types D101, D102, AB-8, DM130, LSA1-0, HPD-100 and DA 201;

4. freezing the macroporous resin adsorption separation liquid obtained in the step (3) to-25 to-5 ℃ (preferably-20 to-15 ℃, then placing the separation liquid in a negative pressure environment with the pressure of-0.07 to-0.03 MPa and the temperature of 10 to 40 ℃ (preferably 20 to 30 ℃) for vacuum extraction for 3 to 8 hours (preferably 5 to 6 hours), condensing gaseous substances generated in the extraction process by a condenser, and collecting condensate;

5. filtering the condensate obtained in the step 4 by using a precision filter of 2-5 microns to obtain filtrate;

6. and (4) sterilizing the filtrate obtained in the step (5) at the ultrahigh pressure of 100-600 Mpa (preferably 350-600 Mpa) at room temperature to obtain the micro-molecular plant cell sap.

The method of the present invention is applied in preparing cosmetics as the water substitute.

The invention has the beneficial effects that:

1. the micro-molecular plant cell sap prepared by the method has higher effective components and heat-sensitive components than the common plant pure dew cell sap, and has better skin permeation effect and absorption rate and good moisturizing effect compared with other similar products.

Note: the production process of the common plant hydrosol comprises the following steps: putting 1 part of plant raw material into production equipment, adding 3-8 parts of water according to a proportion, heating and boiling under normal temperature and pressure (the temperature is high, the heat-sensitive active ingredients are easy to inactivate), condensing generated steam through a condenser, and collecting condensate to obtain the hydrolat.

2. Compared with the existing method for extracting the common pure dew cell sap, the method is a non-distillation method, does not use steam in the production and preparation process, can reduce the use of fuels such as natural gas, coal and the like, and reduces the environmental pollution generated by combustion waste gas.

3. The micro-molecular cell sap prepared by the method is used as a substitute of water in cosmetic raw materials, contains rich plant polysaccharide components, retains natural fragrance of plants, has very good moisture retention property, and realizes a product 'anhydrous formula'.

The product obtained by the method is micro-molecular cell sap, is light in color, has the most effective components of volatile small-molecular compounds, has good retention of heat-sensitive active components, and can be widely applied to daily chemical products such as cosmetics, foods and the like.

Drawings

FIG. 1 is an HPLC chromatogram of a New suona I standard from example 2.

FIG. 2 is an HPLC chromatogram of New suona I lot number 20220501 in example 2.

FIG. 3 is an HPLC chromatogram of New suona I lot number 20220502 in example 2.

FIG. 4 is an HPLC chromatogram of New suona I lot number 20220503 in example 2.

FIG. 5 is an HPLC chromatogram of New suona I lot number 20220504 in example 2.

FIG. 6 is an HPLC plot of New suona sin I lot No. 20220505 of example 2.

The abscissa of fig. 1 to 6 represents time (in min); the ordinate is peak height/absorption intensity (in mv).

Detailed Description

Example 1. A series of comparative experiments were performed including the low temperature extraction of micro-clusters of water of the invention compared to non-low temperature extraction, and the low temperature extraction of micro-clusters of water of the invention compared to low temperature extraction of plain water, with the results shown in table 1.

In the comparison test of the low-temperature extraction of the micro-molecular cluster water and the low-temperature extraction of the common water, for the extraction process of the same plant, only the difference between the micro-molecular cluster water and the common water exists, and other steps and process conditions are completely the same.

Each comparative experiment involved an extraction process of:

1. taking 1 part by weight of plant tissues related to test contents, adding 6 parts by weight of micro-molecular group water, and soaking and extracting for 5 hours at normal temperature and normal pressure;

2. filtering with a 100-mesh screen to obtain a coarse extraction solution;

3. introducing the crude extraction liquid obtained in the step 2 into a macroporous adsorption resin column for adsorption, performing desorption separation by using micro molecular group water with the volume of 5 columns, and collecting effluent liquid to obtain macroporous adsorption separation liquid, wherein the types of the macroporous resin are D101, D102, AB-8, DM130 and LSA1-0 respectively;

4. freezing the macroporous resin adsorption separation liquid obtained in the step (3) to-22 ℃, and then placing the liquid in a negative pressure environment with the pressure of-0.06 MPa and the temperature of 27 ℃ for vacuum extraction for 6 hours; condensing gaseous substances generated in the extraction process at low temperature by a condenser, and collecting condensate;

5. filtering the condensate obtained in the step 4 by using a precision filter with the size of 3 microns to obtain filtrate;

6. and (4) sterilizing the filtrate obtained in the step (5) at ultrahigh pressure and room temperature, wherein the ultrahigh pressure is 400Mpa, and thus obtaining the corresponding micro-molecular plant cell sap in the table 1.

The results in Table 1 show that the content of heat-sensitive active ingredients in the micro-molecular plant cell sap was much higher under the same conditions than under the high temperature conditions.

The results in table 1 also show that the thermosensitive active ingredient content in the plant cell sap, the thermosensitive active ingredient content and the extraction rate of the micro-micelle water extraction were higher than those of the general water extraction under the same conditions.

TABLE 1

Example 2. The test results of the process repeatability and product quality stability of the invention are shown in table 2.

TABLE 2

The results in table 2 show that the technical quality index has good repeatability after repeated pilot scale experiments of multiple pilot scale experiments on the completely same raw materials and process conditions, and can be applied to industrial production.

The extraction process for each lot product in table 2 is:

1. taking 1 part by weight of fresh rose flowers, adding 4 parts of micro molecular group water according to the weight ratio, and soaking and extracting for 4 hours at 20 ℃ and normal pressure;

2. filtering with a 120-mesh screen to obtain a coarse extraction solution;

3. introducing the crude extraction liquid obtained in the step 2 into a macroporous adsorption resin column for adsorption, performing desorption separation by using micro molecular group water with the volume of 5 columns, and collecting effluent liquid to obtain a macroporous adsorption resin separation liquid, wherein the macroporous resin is a mixture of types D102, DM130, HPD-100 and DA 201;

4. freezing the macroporous resin adsorption separation liquid obtained in the step (3) to-20 ℃, and then placing the liquid in a negative pressure environment with the pressure of-0.06 MPa and the temperature of 25 ℃ for vacuum extraction for 5 hours; condensing gaseous substances generated in the extraction process at low temperature by a condenser, and collecting condensate;

5. filtering the condensate obtained in the step 4 by using a 5-micron precision filter to obtain filtrate;

6. and (5) sterilizing the filtrate obtained in the step (5) at ultrahigh pressure and room temperature, wherein the ultrahigh pressure is 400Mpa, and thus obtaining the micro-molecular plant cell sap of the batch number.

The heat-sensitive active ingredient contents described in tables 1 and 2 are weight percentage contents (calculated as dry product).

Claims

1. A preparation method of micro-molecular plant cell sap is characterized by comprising the following steps:

(1) Taking one or more of fresh flowers, stems, leaves and root blocks of plants, adding 3-6 parts of micro molecular group water according to the weight ratio, and soaking and extracting for 4-6 hours at normal temperature and normal pressure;

(2) Filtering by using a 100-200 mesh screen to obtain a coarse extraction solution;

(3) Introducing the crude extraction liquid obtained in the step (2) into a macroporous adsorption resin column for adsorption, performing desorption separation by using micromolecular water with the volume of 3-5 columns, and collecting effluent liquid to obtain a macroporous adsorption resin separation liquid, wherein the macroporous resin is one or a mixture of types D101, D102, AB-8, DM130, LSA1-0, HPD-100 and DA 201;

(4) Freezing the macroporous resin adsorption separation liquid obtained in the step (3) to-25 ℃ to-5 ℃, and then placing the liquid in a negative pressure environment with the pressure of-0.07 to-0.03 MPa and the temperature of 10 to 40 ℃ for vacuum extraction for 3 to 8 hours; condensing gaseous substances generated in the extraction process by a condenser, and collecting condensate;

(5) Filtering the condensate obtained in the step (4) by using a precision filter of 2-5 microns to obtain filtrate;

(6) And (4) sterilizing the filtrate obtained in the step (5) at ultrahigh pressure and room temperature, wherein the ultrahigh pressure is 100-600 Mpa, and thus obtaining the micro-molecular plant cell sap.

2. The method of claim 1, wherein the temperature of the separated liquid in step (4) is-20 to-15 ℃.

3. The method of producing micro-molecular plant cell sap as claimed in claim 1, wherein: the temperature of the vacuum extraction in the step (4) is 20-30 ℃, and the time is 5-6 h.

4. The method of producing micro-molecular plant cell sap as claimed in claim 1, wherein: the ultra-high pressure in the step (6) is 350-600 Mpa.

5. The application of the preparation method of micro-molecular plant cell sap is characterized in that: the obtained micro-molecular plant cell sap can be used as substitute for water to prepare cosmetic.