CN112957297A

CN112957297A - Nicandra physaloides seed natural skin-care hand sanitizer and preparation method thereof

Info

Publication number: CN112957297A
Application number: CN202110329925.0A
Authority: CN
Inventors: 罗书勤; 李海英; 张洁
Original assignee: Hefei Dongjian New Material Technology Co ltd
Current assignee: Hefei Dongjian New Material Technology Co ltd
Priority date: 2021-03-29
Filing date: 2021-03-29
Publication date: 2021-06-15

Abstract

The invention discloses a natural skin-care hand sanitizer containing nicandra physaloides seeds and a preparation method thereof. The natural skin care hand sanitizer containing nicandra physaloides seeds comprises the following raw materials: nicandra physaloides seed composite microcapsule, hyaluronic acid, sodium cocoyl glycinate, lauramidopropyl hydroxysultaine, phenoxyethanol and water. The natural nicandra physaloides seed skin care hand sanitizer can effectively clean skin, can make the skin touch smooth after use, has the effects of long-acting bacteriostasis, whitening, moisture retention and the like, and has stable performance.

Description

Nicandra physaloides seed natural skin-care hand sanitizer and preparation method thereof

Technical Field

The invention belongs to the field of daily chemical products, and particularly relates to a natural nicandra physaloides seed skin-care hand sanitizer and a preparation method thereof.

Background

Nicandra physaloides seed, Latin's scientific name: nicandrapysalodes, native to Peru, are plants of the genus Nicandra of the family Solanaceae, and are widely distributed in Yunnan, Guangxi, Sichuan, Guizhou and other places in the southwest region of China, and the northern region is also artificially cultivated. The Nicandra physaloides seeds are seeds of Nicandra physaloides, are main raw materials for making famous snack ice powder by people in southwest regions, are low in price, and the price of the prepared snack ice powder is low. The surface of the Nicandra physaloides seed is brown, and the particle size is about 1.5 mm; the colloidal material is a unique composite macromolecular polysaccharide structure, can quickly form hydrogen bonds when combined with water, shows strong sol, thickening and stable physical characteristics, has a good water-retaining effect, and has the effects of clearing heat, annealing, dispelling wind, diminishing inflammation and the like.

The nicandra physaloides seed extract is mainly applied to the aspects of food preservation, beverage thickening and traditional Chinese medicine health care, and the researches on other aspects are few. Patent CN109288812A "A preparation method of Nicandra physaloides Gum microspheres" discloses a preparation method of Nicandra physaloides Gum microspheres, which prepares a Nicandra physaloides polysaccharide solution, a calcium chloride solution and a liquid medicine into Nicandra physaloides Gum microspheres by a dropping method, and has the advantages of simple and high-efficiency method, good encapsulation efficiency, drug-loading rate and slow-release effect. The application of the nicandra physaloides seed extract to the field of daily chemicals is few, and the nicandra physaloides seed extract is mainly used for preparing facial masks. Patent CN107753403A 'A Natural Nutrition moisture mask and preparation method thereof' discloses an application of Nicandra physaloides seed in the technical field of beauty and skin care, and the Nicandra physaloides polysaccharide is used as a structural support of the mask and plays a role in water retention and water supplement.

How to accurately position the structure and the efficacy characteristics of the nicandra physaloides seed extract, providing a new direction for the application of the nicandra physaloides seed extract and improving the added value of the nicandra physaloides seed extract.

Disclosure of Invention

In order to solve the problems in the prior art, the invention provides a natural nicandra physaloides seed skin-care hand sanitizer and a preparation method thereof.

The invention is realized by the following steps:

the natural skin-care hand sanitizer containing nicandra physaloides seeds comprises the following components in parts by weight: 5-10 parts of nicandra physaloides seed composite microcapsule, 1-3 parts of hyaluronic acid, 5-10 parts of sodium cocoyl glycinate, 8-15 parts of lauramidopropyl hydroxysulfobetaine, 0.02-0.1 part of phenoxyethanol and the balance of water, wherein the sum of the parts by weight of the components is 100.

The preparation method of the nicandra physaloides seed composite microcapsule comprises the following steps:

s1, preparing a preparation solution: adding grape seed procyanidin into water, wherein the material-liquid ratio is 1g (1-3) mL, stirring at 100-500rpm for 2-8min to obtain a mixed solution I, and mixing the mixed solution I and the nicandra physaloides seed extracting solution according to the volume ratio of 1: (1-3) mixing, stirring at 500rpm for 2-8min at 100-;

s2, dripping gel: controlling the flow rate of the prepared liquid A to be 7-12mL/min by using a microcapsule granulator, spraying a gel through a spray nozzle with the aperture of 0.45mm to obtain the gel containing gel balls, wherein the spray nozzle is 6cm away from the liquid surface of the gel, and controlling the spraying time of the prepared liquid A so that the volume ratio of the sprayed prepared liquid A to the volume of the gel is 1: (8-20);

s3, cold setting and drying: standing the gel containing the gel balls at 4 ℃ for 12-24h, filtering, washing with clear water, collecting the gel balls, absorbing moisture on the surfaces of the gel balls by filter paper, and drying at 55-65 ℃ for 24h to obtain the nicandra physaloides seed composite microcapsules.

The gel is at least one of a magnesium ascorbyl phosphate solution and a calcium chloride solution.

As a preferable technical scheme of the invention, the gel is prepared by mixing 8-12 wt% of magnesium ascorbyl phosphate solution and 3-6 wt% of calcium chloride solution according to the volume ratio of 1: (1-5).

The preparation method of the nicandra physaloides seed extracting solution comprises the following steps:

placing the nicandra physaloides seeds into water, stirring for 5-10min at 30-50 ℃ under the assistance of (400-800) W/(25-40) kHz ultrasonic wave, wherein the material-liquid ratio is 1g: (10-30) mL, stirring speed of 100-400 rpm. Separating liquid phase and solid phase with separator after stirring, and collecting liquid phase to obtain herba Nicandrae Physaloidis seed extractive solution.

Pectin in the nicandra physaloides seed extract has the characteristics of high-ester pectin and low-ester pectin, a large molecular chain of the pectin is connected with a plurality of hydrophilic groups, calcium and magnesium ions are added to be chelated with oxygen atoms on the hydrophilic groups to occupy hydrophilic space, so that an egg lattice structure is formed, the molecular chains of the pectin are combined more tightly, and gel is formed. When the preparation liquid A is sprayed into the gel, pectin molecules in the nicandra physaloides seed extract are contacted with calcium and magnesium ions, the surface of the nicandra physaloides seed extract is immediately gelled to form a spherical shape, and then solid gel spheres are gradually formed along with the penetration of the calcium and magnesium ions. Experiments show that gel balls cannot be effectively obtained when the concentration of the nicandra physaloides seed extract or the gelling agent is low, and microcapsules obtained are too hard when the concentration of the nicandra physaloides seed extract or the gelling agent is high, so that active ingredients cannot be effectively released when the hand sanitizer is used, and the effect is influenced. When 3-6 wt% calcium chloride solution is used as a gel independently, the gel ball forming speed is fastest; when 8-12 wt% magnesium ascorbyl phosphate is used alone as a gelling agent, the gel sphere formation speed is slowest. When the calcium chloride solution with the weight percentage of 3-6 percent and the magnesium ascorbyl phosphate solution with the weight percentage of 8-12 percent are used together according to a certain proportion, the gel speed is moderate. For the embedded core material grape seed procyanidin, not only can more effective protection and slow release be obtained, but also the ascorbic acid decomposed by the magnesium ascorbyl phosphate and the grape seed procyanidin have synergistic antioxidant effect. Improves the stability and skin care performance of the natural skin care hand sanitizer containing nicandra physaloides seeds.

As a preferred technical scheme, the preparation method of the nicandra physaloides seed composite microcapsule comprises the following steps:

s1, preparing a preparation solution: adding grape seed procyanidin into montmorillonite microemulsion with a material-liquid ratio of 1g (1-3) mL and stirring at 100-one 500rpm for 2-8min to obtain a mixed solution I, and mixing the mixed solution I and the nicandra physaloides seed extracting solution in a volume ratio of 1: (1-3) mixing, stirring at 500rpm for 2-8min at 100-;

s2, dripping gel: controlling the flow rate of the prepared liquid A to be 7-12mL/min by using a microcapsule granulator, spraying a gel through a spray nozzle with the aperture of 0.45mm to obtain the gel containing gel balls, wherein the spray nozzle is 6cm away from the liquid surface of the gel, and controlling the spraying time of the prepared liquid A so that the volume of the sprayed prepared liquid A and the volume of the gel are in a ratio of 1: (8-20);

The preparation method of the montmorillonite microemulsion comprises the following steps:

s1, purification: montmorillonite and water were mixed at a ratio of 1g: (20-40) mixing the materials in a material-liquid ratio, standing for 2-3 days, then sieving with a 200-mesh vibrating screen at a stirring speed of 100-200rpm, and deslagging by a deslagging cyclone to obtain montmorillonite emulsion;

s2, ultramicro treatment: adding sodium carbonate 2-5 wt% of the montmorillonite emulsion and concentrated sulfuric acid 90-95 wt% of the montmorillonite emulsion 0.5-1.5 wt% of the montmorillonite emulsion into the montmorillonite emulsion at room temperature, and performing ultramicro treatment in an ultrasonic micromanipulator for 20-35min to obtain the montmorillonite microemulsion.

Montmorillonite is a natural mineral of silicate, expands several times after absorbing water, has good dispersibility, viscosity, lubricity, thermal stability, higher hot and wet compressive strength and compressive strength, and also has strong adsorption capacity and cation exchange performance. When the prepared liquid A is sprayed into the gel, the pectin and the calcium and magnesium ions form gel, and simultaneously, the calcium and magnesium ions are adsorbed by the montmorillonite and intercalated into the montmorillonite interlayer through ion exchange, so that the montmorillonite and the gel structure are combined in a staggered manner to form the composite microcapsule wall material. The stability, slow release performance, mechanical performance and skin feel of the microcapsule are improved by adding a proper amount of montmorillonite microemulsion.

The invention also provides a preparation method of the natural skin-care hand sanitizer containing nicandra physaloides seeds, which comprises the following steps:

mixing nicandra physaloides seed composite microcapsule, hyaluronic acid, sodium cocoyl glycinate, lauramidopropyl hydroxysulfobetaine, phenoxyethanol and water in proportion, stirring at the speed of 300rpm under the heating condition of 60-80 ℃ for 10-40min, and naturally cooling to room temperature to obtain the nicandra physaloides seed composite microcapsule.

Has the advantages that: (1) the invention provides a preparation method of nicandra physaloides seed composite microcapsules, which has the advantages of low raw material price, simple preparation steps and easy operation; the montmorillonite microemulsion is creatively added in the preparation process, and the stability, the embedding rate and the mechanical property of the composite microcapsule are effectively improved through the synergistic effect among the components; (2) the provided natural skin care hand sanitizer containing nicandra physaloides seeds can effectively clean skin, can make skin feel smooth after being used, has the effects of whitening, moisturizing and the like, and is stable in performance.

Detailed Description

The raw materials used in the examples were as follows:

montmorillonite, available from Suoguang Midijie montmorillonite Co., Ltd., having a purity of 90% and a particle size of 325 mesh.

Nicandra physaloides seed is commercially available.

Grape seed procyanidin with a purity of 95% was purchased from Xian Jinkuifang plant technology development Co., Ltd.

Magnesium ascorbyl phosphate, CAS No.: 113170-55-1, available from Wuhan eosin Biotechnology, Inc.

Hyaluronic acid, CAS No.: 9004-61-9.

Cocoyl sodium glycinate, CAS No.: 90387-74-9.

Lauramidopropyl hydroxysultaine, available from Suzhou Yuntan chemical Co.

Phenoxyethanol, CAS No.: 122-99-6.

Calcium chloride, CAS number: 10043-52-4.

Example 1

The natural skin care hand sanitizer containing nicandra physaloides seeds comprises the following components in parts by weight: 8 parts of nicandra physaloides seed composite microcapsule, 2 parts of hyaluronic acid, 8 parts of sodium cocoyl glycinate, 10 parts of lauramidopropyl hydroxysulfobetaine, 0.05 part of phenoxyethanol and 71.95 parts of water.

s1, preparing a preparation solution: adding grape seed procyanidin into montmorillonite microemulsion with a material-liquid ratio of 1g:2mL, stirring at 300rpm for 5min to obtain a mixed solution I, and mixing the mixed solution I and the nicandra physaloides seed extract in a volume ratio of 1: 2, mixing and stirring at 200rpm for 4min to obtain a prepared solution A;

s2, dripping gel: controlling the flow rate of the prepared liquid A to be 10mL/min by using a microcapsule granulator, spraying the prepared liquid A into the gel through a spray nozzle with the aperture of 0.45mm to obtain the gel containing gel balls, wherein the spray nozzle is 6cm away from the liquid surface of the gel, and controlling the spraying time of the prepared liquid A so that the volume of the sprayed prepared liquid A and the volume of the gel are in a ratio of 1: 10;

s3, cold setting and drying: standing the gel containing the gel balls at 4 ℃ for 18h, filtering, washing with water, collecting the gel balls, absorbing moisture on the surfaces of the gel balls by filter paper, and drying at 55 ℃ for 24h to obtain the nicandra physaloides seed composite microcapsules.

The gel is prepared from 10 wt% magnesium ascorbyl phosphate solution and 4 wt% calcium chloride solution according to the volume ratio of 1: 2.

s1, purification: montmorillonite and water were mixed at a ratio of 1g: mixing 30mL of materials and liquid, standing for 2.5 days, sieving by a 200-mesh vibrating screen at a stirring speed of 100rpm, and deslagging by a deslagging cyclone to obtain montmorillonite emulsion;

s2, ultramicro treatment: adding sodium carbonate 3 wt% of the montmorillonite emulsion and concentrated sulfuric acid 92 wt% of the montmorillonite emulsion 1 wt% into the montmorillonite emulsion at room temperature, and performing ultramicro treatment in an ultrasonic micromanipulator for 30min to obtain montmorillonite microemulsion.

putting the nicandra physaloides seeds into water, stirring for 8min at 40 ℃ under the assistance of 400W/30kHz ultrasonic waves, wherein the material-liquid ratio is 1g: 20mL, with a stirring speed of 200 rpm. Separating liquid phase and solid phase with separator after stirring, and collecting liquid phase to obtain herba Nicandrae Physaloidis seed extractive solution.

A preparation method of a natural skin care hand sanitizer containing nicandra physaloides seeds comprises the following steps:

mixing nicandra physaloides seed composite microcapsule, hyaluronic acid, sodium cocoyl glycinate, lauramidopropyl hydroxysulfobetaine, phenoxyethanol and water in proportion, stirring at 150rpm for 20min under the heating condition of 65 ℃, and naturally cooling to room temperature to obtain the nicandra physaloides seed composite microcapsule.

Example 2

s1, preparing a preparation solution: adding grape seed procyanidin into water at a material-liquid ratio of 1g:2mL, stirring at 300rpm for 5min to obtain a mixed solution I, mixing the mixed solution I and the nicandra physaloides seed extracting solution in a volume ratio of 1: 2, mixing and stirring at 200rpm for 4min to obtain a prepared solution A;

s2, dripping gel: controlling the flow rate of the prepared liquid A to be 10mL/min by using a microcapsule granulator, spraying a gel through a spray nozzle with the aperture of 0.45mm to obtain the gel containing gel balls, wherein the spray nozzle is 6cm away from the liquid surface of the gel, and controlling the spraying time of the prepared liquid A so that the volume ratio of the sprayed prepared liquid A to the volume of the gel is 1: 10;

s3, cold setting and drying: standing the gel containing the gel balls at 4 ℃ for 18h, filtering, washing with clear water, collecting the gel balls, absorbing moisture on the surfaces of the gel balls by filter paper, and drying at 55 ℃ for 24h to obtain the nicandra physaloides seed composite microcapsules.

Example 3

The gel is 10 wt% magnesium ascorbyl phosphate solution.

Example 4

The gel is a 4 wt% calcium chloride solution.

Comparative example 1

s2, drying: and (4) freeze-drying the prepared solution A to obtain the nicandra physaloides seed composite microcapsule.

Comparative example 1

The aloe vera bacteriostatic hand sanitizer is purchased in the market.

Test example 1

The examples, comparative examples and comparative examples were tested for cleaning effect by referring to the method for measuring oil removal rate in "manual dishwashing detergent" GB 9985-.

Table 1: cleaning effect test table for hand sanitizer

	Oil removal rate/%)
		Example 1	87.40
Example 2	85.62
		Example 3	84.34
Example 4	84.73
		Comparative example 1	81.95
Comparative example 1	84.05

The oil removal rate of each example is equivalent, and the oil removal rate of example 1 is superior to that of the commercial hand sanitizer. The montmorillonite has strong adsorbability, can effectively improve the cleaning effect, has the characteristic of low-foam decontamination, enables the hand sanitizer to be decontaminated efficiently and to be easier to wash, and reduces residues. Comparative example 1 the hand sanitizer added with the nicandra physaloides seed microcapsule prepared by the freeze-drying method absorbs water to swell to form viscous gel, so that the washing difficulty is increased, residues are easy to occur, and the cleaning effect is low.

Test example 2

The stability of the natural skin-care hand sanitizer of the pseudo-wintercherry seeds in each example is tested according to QB 2654-2004-hand sanitizer.

(1) Heat resistance test: samples in the examples are placed in an incubator (40 +/-1) DEG C and kept for 24h, and after being taken out and returned to the room temperature, whether the samples are discolored, layered and peculiar, and whether transparent samples are turbid or not are observed.

(2) Cold resistance test: the samples of the examples are placed in a refrigerator at (-5 +/-2) DEG C for 24h, taken out and restored to room temperature for comparison, and whether the samples are discolored and layered or not and whether the transparent samples are turbid or not are observed.

The method is characterized in that the phenomena of color change, layering, odor turbidity change and the like of a test sample are graded, and the grading is 0-3 grades, wherein the 0 grade is the phenomena of no color change, layering, odor and turbidity, the 1 grade is the phenomena of slight color change, layering, odor and turbidity, the 2 grade is the phenomena of slight color change, layering, odor and turbidity, and the 3 grade is the phenomena of obvious color change, layering, odor and turbidity. The test results are shown in Table 2.

Table 2: nicandra physaloides seed natural skin care hand sanitizer stability test table

	Stability against Heat	Stability against cold
			Example 1	Level 0	Level 0
Example 2	Level 0	Level 0
			Example 3	Level 0	Level 0
Example 4	Level 1	Level 0
			Comparative example 1	Stage 2	Stage 2
Comparative example 1	Level 0	Level 0

Grape seed procyanidin has activities of resisting oxidation, resisting bacteria, whitening, preserving moisture and the like, but is unstable in structure and easy to discolor and separate out due to the influence of environmental conditions. The active component grape seed procyanidin in the natural skin care hand sanitizer containing nicandra physaloides seeds is embedded in nicandra physaloides seed microcapsules, so that the stability can be effectively improved. Comparative example 1 the nicandra physaloides seed microcapsule prepared by the freeze-drying method is added into the hand sanitizer, and then absorbs water to swell to form viscous gel, so that the grape seed procyanidin as an embedding substance is easily released into the hand sanitizer in a short time, and the color becomes dark due to the fact that the procyanidin is easily oxidized and condensed when being heated in a weak alkaline environment of the hand sanitizer; at lower temperatures, the viscous gel tends to clump together, causing the hand sanitizer to delaminate. In examples 1-4, the gel and the nicandra physaloides seed extract are adopted to form the stable gel ball microcapsule, and the gel in examples 1-3 contains the magnesium ascorbyl phosphate solution, because the magnesium ascorbyl phosphate can be decomposed to generate ascorbic acid, the reducibility of the magnesium ascorbyl phosphate can further protect grape seed procyanidin, the stability of the hand sanitizer is improved, and the stability is better.

Test example 3

The bacteriostatic performance of the natural skin care hand sanitizer containing the nicandra physaloides seeds in each example is tested, and the bacteriostatic performance is tested by adopting a bacteriostatic effect test method, namely a retention method, of bacteriostatic human skin cleaning products according to the QB/T2738-2005 evaluation method of the antibacterial and bacteriostatic effects of daily chemical products. The antibacterial stability is tested by adopting a method for testing the stability of the antibacterial and bacteriostatic effects of daily chemical products, namely a 14-day accelerated test. The number of tested persons is as follows: the number of people is 20. Strain: staphylococcus aureus (ATCC 27217). The test results are shown in Table 3.

Table 3: nicandra physaloides seed natural skin care hand sanitizer antibacterial performance test table

The nicandra physaloides seed microcapsule prepared in example 1 is added with montmorillonite microemulsion, and calcium and magnesium ions are subjected to ion exchange with montmorillonite and intercalated between montmorillonite in the process of occupying the hydrophilic space of the nicandra physaloides seed extract to form gel, so that the nicandra physaloides seed extract and the montmorillonite are intercrossingly connected, the process of forming the gel is relatively slow, the gel structure is relatively fluffy, and the connection force between the gel structures is stronger. The microcapsule can be fully swelled but not easily broken during storage, and can rapidly and completely release effective components by kneading in the using process, thereby exerting the effects of resisting and inhibiting bacteria, whitening, moisturizing and whitening by ascorbic acid of the grape seed procyanidin. In addition, the montmorillonite micro-emulsion can improve the delicate and smooth touch of the hand sanitizer, the nicandra physaloides seed extract has film forming property and good moisturizing effect, the touch of the hand skin is smooth after use, and the nicandra physaloides seed also has certain antibacterial and bacteriostatic effects.

The embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.

Claims

1. A natural skin-care hand sanitizer containing nicandra physaloides seeds is characterized by comprising nicandra physaloides seed composite microcapsules.

2. The natural skin care hand sanitizer of nicandra physaloides seed according to claim 1, which comprises the following raw materials: nicandra physaloides seed composite microcapsule, hyaluronic acid, sodium cocoyl glycinate, lauramidopropyl hydroxysultaine, phenoxyethanol and water.

3. The natural skin care hand sanitizer of nicandra physaloides seed according to claim 1, which comprises the following raw materials in parts by weight: 5-10 parts of nicandra physaloides seed composite microcapsule, 1-3 parts of hyaluronic acid, 5-10 parts of sodium cocoyl glycinate, 8-15 parts of lauramidopropyl hydroxysulfobetaine, 0.02-0.1 part of phenoxyethanol and 61.90-80.98 parts of water.

4. The natural nicandra physaloides seed skin care hand sanitizer according to any one of claims 1 to 3, wherein the preparation method of the nicandra physaloides seed composite microcapsule comprises the following steps:

5. The natural nicandra physaloides seed skin care hand sanitizer according to claim 4, wherein the gelling agent is at least one of a magnesium ascorbyl phosphate solution and a calcium chloride solution.

6. The natural nicandra physaloides seed skin care hand sanitizer according to claim 5, wherein the concentration of the magnesium ascorbyl phosphate solution is 8-12 wt%; the concentration of the calcium chloride solution is 3-6 wt%.

7. The natural skin care hand sanitizer of nicandra physaloides seed as claimed in claim 4, wherein the preparation method of the nicandra physaloides seed extract comprises the following steps: placing the nicandra physaloides seeds into water, stirring for 5-10min at 30-50 ℃ under the assistance of (400-800) W/(25-40) kHz ultrasonic wave, wherein the material-liquid ratio is 1g: (10-30) mL, the stirring speed is 100-400 rpm; separating liquid phase and solid phase with separator after stirring, and collecting liquid phase to obtain herba Nicandrae Physaloidis seed extractive solution.

8. The preparation method of the nicandra physaloides seed natural skin care hand sanitizer according to claim 4, wherein the preparation method of the nicandra physaloides seed composite microcapsule comprises the following steps:

9. The nicandra physaloides seed natural skin care hand sanitizer according to claim 8, wherein the montmorillonite microemulsion is prepared by the following steps:

10. The method for preparing the natural skin-care hand sanitizer containing nicandra physaloides seeds as claimed in any one of claims 1 to 9, which comprises the following steps:

mixing nicandra physaloides seed composite microcapsule, hyaluronic acid, sodium cocoyl glycinate, lauramidopropyl hydroxysultaine, phenoxyethanol and water, stirring at the speed of 300rpm under the heating condition of 60-80 ℃ for 10-40min, and naturally cooling to room temperature to obtain the nicandra physaloides seed composite microcapsule.