CN115518030A

CN115518030A - Preparation method of dimethicone cream

Info

Publication number: CN115518030A
Application number: CN202210955713.8A
Authority: CN
Inventors: 李雅玉; 刘萍; 邹小慧; 胡丽娟; 简梁; 赵文卓
Original assignee: Zigong Honghe Pharmaceutical Co ltd
Current assignee: Zigong Honghe Pharmaceutical Co ltd
Priority date: 2022-08-10
Filing date: 2022-08-10
Publication date: 2022-12-27

Abstract

The invention relates to a preparation method of simethicone cream, which comprises the following steps: step one, adding carbomer into purified water, freezing at-20 ℃, and stirring until the carbomer is completely dissolved to obtain carbomer transparent gel; step two, mixing and stirring dimethicone, white vaseline and carbomer transparent gel uniformly to obtain a pre-emulsified gel system; step three, adding sorbic acid and purified water into polyoxyl (40) stearate, and heating until the sorbic acid and the purified water are dissolved to obtain a water phase; step four, adding the water phase into a pre-emulsified gel system, and uniformly stirring to obtain a secondary emulsified paste body; step five, putting the secondary emulsified paste body into a colloid mill for grinding to obtain the simethicone crude cream; and step six, feeding the simethicone crude cream into a homogenizer, and homogenizing at a high speed to obtain the simethicone cream. The product of the invention is oily, fine and smooth, and has small grain size; and the product quality is stable.

Description

Preparation method of dimethicone cream

Technical Field

The invention relates to the technical field of medicinal preparations, in particular to a preparation method of dimethicone cream.

Background

The simethicone is also called methyl silicone oil and polydimethylsiloxane liquid, is a low-molecular-weight liquid polysiloxane structure, and is colorless, tasteless, odorless and nontoxic oily liquid; the molecular formula is CH3[ Si (cH 3) 2] nSi (CH 3) 3, which is widely used for insulating, heat-resisting and moisture-proof filling agents, high-efficiency defoaming agent, release agent, lubricant and surface treating agent. The simethicone is prepared into emulsion or cream to be applied to human skin, has lubricating effect, and has no irritation and easy application.

In pharmacy, different dosage forms are suitable for different medication methods, and compared with emulsion, gel and solution, the cream is more suitable for smooth and hairless skin, diffuse and hyperkeratosis symptoms, palms, soles and other parts; the cream can be oil-in-water (O/W) type or water-in-oil (W/O) type, and the simethicone cream is oil-in-water type, and is a multifunctional cream integrating skin care and skin care when used alone, and simethicone is also commonly used for treating symptoms such as rhagadia, eczema, senile pruritus, etc.

The dimethicone emulsifiable paste is a hospital preparation product recorded in the formulation code of medical institutions in Beijing City published in 2014, and at present, most of products prepared by the existing preparation method of the dimethicone emulsifiable paste have the problems of rough properties, poor stability, inconvenience for transdermal absorption and the like.

Therefore, the method for preparing the simethicone cream can ensure that the prepared simethicone cream product has good properties, stable quality, contribution to transdermal absorption and simple component composition.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provides a preparation method of the dimethicone cream, and the method can ensure that the prepared dimethicone cream has good property and stable quality, is beneficial to transdermal absorption and has simple component composition.

The purpose of the invention is realized by the following technical scheme:

a preparation method of dimethicone cream comprises the following raw materials: 100 parts of dimethicone, 20 parts of white vaseline, 5 parts of carbomer, 100 parts of polyoxyl (40) stearate, 1 part of sorbic acid and 274 parts of purified water;

the preparation method of the simethicone cream comprises the following steps:

a. adding 5 parts of carbomer into 50 parts of purified water, freezing at-20 deg.C, and stirring once every 6min until carbomer is completely dissolved to obtain carbomer transparent gel;

b. mixing and stirring uniformly 100 parts of dimethicone, 20 parts of white vaseline and carbomer transparent gel to obtain a pre-emulsified gel system;

c. adding 1 part of sorbic acid and 224 parts of purified water into 100 parts of polyoxyl (40) stearate, and heating to 100-120 ℃ for dissolution to obtain a water phase;

d. adding the water phase into a pre-emulsified gel system, and uniformly stirring to obtain a secondary emulsified paste body;

e. grinding the secondary emulsified paste body in a colloid mill to obtain the simethicone coarse emulsifiable paste;

f. and (3) feeding the simethicone coarse cream into a homogenizer, and homogenizing at a high speed of 8000-12000 r/min to obtain the simethicone cream.

The main chain of the molecule of the dimeticone is based on Si-O-Si bond, and the side chain is-CH ₃ Side group steric hindrance is small, molecular chain can rotate freely, and simultaneously-CH ₃ and-CH ₃ The interaction force between the silicone oil and the silicone oil is weak, so that the intermolecular force of the silicone oil is weak; the special structure of the molecular composition ensures that the fabric has higher physical and chemical inertness, higher safety in the using process, easy smearing, no pore blockage and no clothes pollution.

Carbomer, also known as a carbonyl ethylene copolymer or carbopol, is a high molecular polymer obtained by crosslinking polyalkylsucrose or polyalkylpentaerythritol with acrylic acid, is white loose powder, and is often used as an auxiliary material in external gels. Carbomers are extremely hydrophilic, dry powders of carbomer are very hygroscopic and when directly added to water or other polar solvents tend to agglomerate or incompletely wet.

Furthermore, the viscosity of the simethicone is 1000cs-1500cs.

The molecular formula of the dimeticone is CH3[ Si (cH 3) 2] nSi (CH 3) 3, the average molecular weight is 5000-100000, and the kinematic viscosity is different from 1.0 multiplied by 10 < -6 > to 100000 multiplied by 10 < -6 > square meters per second according to different molecular weights.

Further, in the step f, the homogenization time is 10-20 minutes, so that the dimethicone cream with reduced viscosity is obtained.

Further, the grinding time in the step e is 0.5 to 1 hour. The colloid mill has dispersing, emulsifying, and homogenizing effects on the paste.

Sorbic acid is a high-efficiency and safe preservative recommended by the international food and agriculture organization and the health organization, and is widely applied to the industries of food, beverage, tobacco, pesticide, cosmetics and the like; the sorbic acid has enhanced acidity due to carbonyl and conjugated double bonds in a sorbic acid molecular structure, and the carbonyl inhibits the growth of microorganisms: the conjugated double bond can be combined with sulfhydryl of microbial enzyme, thereby destroying enzyme system structure, inactivating enzyme, and finally inhibiting microbial propagation to achieve antiseptic and fresh-keeping effects.

Preferably, the mixing and stirring speed in the step b is 600 revolutions per minute, and the mixing and stirring time is 0.5 to 1 hour.

In a specific embodiment of this embodiment, the step a specifically includes: slowly and uniformly adding 5 parts of carbomer into 50 parts of purified water, stirring, putting into a refrigerator, freezing, taking out and stirring once every 6min, wherein the freezing temperature is-20 ℃, and freezing for 30min to obtain carbomer transparent gel.

Polyoxyl (40) stearate is a nonionic surfactant, which is not in an ionic state in solution, has high stability, and is not easily affected by strong electrolyte inorganic salts, acids, and bases. And has good compatibility with other types of surfactants.

Dimethicone and white vaseline are oil phase substances, carbomer transparent gel is mixed with dimethicone and white vaseline to form a pre-emulsification gel system, and carbomer has the double functions of a thickening agent and an emulsifying agent in the process; in the mixing process, the oily substances are observed to be emulsified and disappear, and the viscosity of the mixture is increased, so that a pre-emulsified gel system is obtained; mixing the pre-emulsified gel system with water, further emulsifying by polyoxyl (40) stearate to obtain a secondary emulsified paste body, grinding the secondary emulsified paste body by a colloid mill to obtain the simethicone crude cream, after secondary emulsification and grinding, reducing the viscosity of the simethicone crude cream compared with the pre-emulsified gel system, but still having higher viscosity compared with a cream product, and homogenizing the simethicone crude cream by a homogenizer to reduce the viscosity to obtain the cream product with proper viscosity.

The invention has the beneficial effects that:

(1) In the scheme, the dimeticone, the white vaseline and the carbomer transparent gel are preferentially mixed and emulsified to obtain a pre-emulsified gel system, then the pre-emulsified gel system is mixed with water phase prepared from polyoxyl (40) stearate, sorbic acid and purified water, and finally grinding and homogenizing are carried out to prepare the stable dimeticone cream, namely, the dimeticone, the white vaseline and the carbomer gel are firstly preliminarily emulsified to form the pre-emulsified gel system, then the pre-emulsified gel system is secondarily emulsified through polyoxyl (40) stearate to obtain a cream product with a complex emulsified state, and finally the cream product with reliable quality, stable chemical performance and granularity reaching 2-3 mu m is obtained after the viscosity is adjusted through mechanical acting force;

(2) The carbomer and the polyoxyl (40) stearate have good compatibility, and the carbomer and the polyoxyl (40) stearate are matched for use, so that the cream subjected to high-speed shearing still has good stability while having a proper viscosity property, and can still keep stable after being placed for 3 months under the conditions that the temperature is 30 +/-2 ℃ and the relative humidity is 60 +/-5%, demulsification is not generated, and the particle size is not changed, so that a dimethicone cream product which has good product property and stable quality and is beneficial to transdermal absorption can be prepared by the scheme;

(3) The formula of the scheme is simple in components, and the used raw materials are safe, so that the allergy symptom can be avoided; the dimethicone cream prepared by the scheme is an acidic cream and is suitable for human skin, the sorbic acid action bacteriostatic agent is added, the dimethicone cream is safe and reliable, and the bacteriostatic effect of sorbic acid in the acidic cream is enhanced, so that the dimethicone cream prepared by the scheme has a good bacteriostatic effect, is suitable for skin, and can be stably stored for a long time.

Drawings

FIG. 1 is a schematic representation of the dimethicone cream prepared in example 1;

FIG. 2 is a schematic representation of the dimethicone cream prepared in example 2;

FIG. 3 is a schematic representation of the dimethicone cream prepared in example 3;

FIG. 4 is a schematic of the dimethicone cream prepared in comparative example 1;

FIG. 5 is a schematic of the dimethicone cream prepared in comparative example 2;

FIG. 6 is a schematic view of example 1 after 3 months of storage;

FIG. 7 is a schematic view of example 2 after 3 months of storage;

FIG. 8 is a schematic view of example 3 after 3 months of storage;

FIG. 9 is a schematic view of comparative example 1 after standing for 3 months;

fig. 10 is a schematic view of comparative example 2 after standing for 3 months.

Detailed Description

The technical solution of the present invention is further described in detail with reference to the following specific examples, but the scope of the present invention is not limited to the following.

Example 1

A method for preparing dimethicone cream comprises the following steps:

(1) Adding 5g carbomer into 50g purified water, stirring, freezing in refrigerator, and stirring once every 6min until carbomer is completely dissolved to obtain carbomer transparent gel;

(2) Mixing 100g of dimethicone, 20g of white vaseline and carbomer transparent gel, stirring for 0.5 hour at a stirring speed of 600 min/r, and stirring to obtain a pre-emulsification system;

(3) Adding 1g sorbic acid and 224g purified water into 100g polyoxyl (40) stearate, and heating to 100 ℃ to dissolve to obtain a water phase;

(4) Slowly adding the water phase into the pre-emulsified gel system, and uniformly stirring to obtain a secondary emulsified paste body;

(5) Grinding the secondary emulsified paste body in a colloid mill for 0.5 hour by utilizing the shearing force of the colloid mill to form the simethicone coarse cream;

(6) Homogenizing the simethicone crude cream in a homogenizer at high speed, 8000 rpm, 10 minutes to obtain the simethicone cream.

Wherein the viscosity of the dimeticone is 1000cs.

Further, the step (1) is specifically as follows: slowly and uniformly adding 5g of carbomer into 50g of purified water, stirring, putting into a refrigerator, freezing, taking out and stirring once every 6min, wherein the freezing temperature is-20 ℃, and freezing for 30min to obtain carbomer transparent gel.

The dimethicone cream obtained in this example exhibited the pH of 5 as shown in fig. 1.

Example 2

A method for preparing simethicone cream comprises the following steps:

(1) Adding 5g of carbomer into 50g of purified water, stirring, freezing in a refrigerator, taking out every 6min, and stirring once until the carbomer is completely dissolved to obtain carbomer transparent gel;

(2) Mixing 100g of dimethicone, 20g of white vaseline and carbomer transparent gel, stirring for 40 minutes at a stirring speed of 600 min/r, and stirring uniformly to obtain a pre-emulsification system;

(3) Adding 1g sorbic acid and 224g purified water into 100g polyoxyl (40) stearate, and heating to 110 ℃ to dissolve to obtain a water phase;

(5) Grinding the secondary emulsified paste body in a colloid mill for 40 minutes by utilizing the shearing force of the colloid mill to ensure that the aqueous phase is fused with the pre-emulsified gel system to form the simethicone coarse emulsifiable paste;

(6) Homogenizing the simethicone crude cream in homogenizer at high speed, 10000 rpm, 15 minutes to obtain the simethicone cream shown in figure 2.

Wherein the viscosity of the dimeticone is 1000cs.

Further, the step (1) is specifically as follows: slowly and uniformly spreading 5g of carbomer into 50g of purified water, stirring, putting into a refrigerator, freezing, taking out and stirring once every 6min, wherein the freezing temperature is-20 ℃, and freezing for 30min to obtain carbomer transparent gel.

Example 3

A method for preparing dimethicone cream comprises the following steps:

(2) Mixing 100g of dimethicone, 20g of white vaseline and carbomer transparent gel, stirring for 50 minutes at a stirring speed of 600 min/r, and stirring uniformly to obtain a pre-emulsification system;

(3) Adding 1g sorbic acid and 224g purified water into 100g polyoxyl (40) stearate, and heating to 120 ℃ to dissolve to obtain a water phase;

(5) Grinding the secondary emulsified paste body in a colloid mill for 50 minutes by utilizing the shearing force of the colloid mill to ensure that the aqueous phase is fused with the pre-emulsified gel system to form the simethicone crude cream;

(6) Homogenizing the simethicone crude cream in a homogenizer at high speed of 12000 r/min for 20 minutes to obtain the simethicone cream shown in figure 3.

Wherein the viscosity of the dimeticone is 1500cs.

Comparative example 1

The composition and the process flow of the preparation method of the product in the comparative example are the same as those in example 1, and the difference is that the process parameters of the comparative example are the same as those of the existing preparation method of the simethicone cream, and a homogenizer is not adopted for homogenization.

(1) Adding 5g carbomer into 50g purified water, stirring, freezing in a refrigerator at-20 deg.C, taking out every 6min, stirring once, and dissolving carbomer completely after 30min to obtain carbomer transparent gel;

(2) Mixing 1000cs of dimethicone 100g, white vaseline 20g and carbomer transparent gel, stirring for 50 minutes at a stirring speed of 600 min/r, and stirring to obtain a pre-emulsification system;

(3) Adding 1g sorbic acid and 224g purified water into 100g polyoxyl (40) stearate, and heating to 70 ℃ to dissolve to obtain a water phase;

(5) And (3) putting the secondary emulsified paste body into a colloid mill for grinding, grinding for 30 minutes by utilizing the shearing force of the colloid mill, and fusing the aqueous phase and the pre-emulsified gel system to obtain the dimeticone cream shown in the figure 4.

Comparative example 2

The composition of the product of this comparative example was the same as the preparation of the existing dimethicone cream, as shown in table 1, and the preparation of this comparative example was the same as example 1.

(1) Mixing 1000cs dimethicone with stearic acid, lanolin and white vaseline for 50 min at 600 min/r to obtain oil phase;

(2) Directly adding appropriate amount of purified water into ethylparaben, triethanolamine and glycerol to 200ml, heating to 100 deg.C, dissolving and stirring to form water phase;

(3) Slowly adding the water phase into the oil phase, grinding with a colloid mill for 30min by using the shearing force of the colloid mill to fuse the water phase and the oil phase to form the simethicone coarse cream;

(4) Homogenizing the crude dimethicone cream in homogenizer at high speed at 8000 rpm for 10 min to obtain dimethicone cream shown in figure 5.

TABLE 1 product composition

Material(s)

Dimethicone

Stearic acid

Lanolin

White vaseline

Hydroxyphenyl Ethyl ester

Triethanolamine

Glycerol

Purified water

Dosage (g)

100g

74.5g

10g

35g

0.5g

10g

20g

250g

Examples of the experiments

And (3) comparing detection results of the dimethicone cream product:

1. the simethicone creams prepared in example 1, example 2, example 3, comparative example 1 and comparative example 2 were sampled, smeared and observed under a microscope for the particle size of the formulated product:

(1) Example 1 the prepared product has oily and fine properties; the particle size is generally 1 μm and 2-4 μm larger when observed under a microscope;

(2) Example 2 the prepared product has oily and fine properties; the particle size is generally 1 μm and larger is 2-3 μm when observed under a microscope;

(3) Example 3 the prepared product has oily and fine properties; the particle size is generally 1 μm and 2-3 μm larger when observed under a microscope;

(4) The prepared product of the comparative example 1 has uneven properties, particles and incomplete emulsification; the particle size is 30-35 μm and 40-50 μm larger under microscope observation;

(5) The prepared product has fine and smooth properties and incomplete emulsification in a comparative example 2; particle sizes of 3-4 μm, and more typically 5-7 μm, were observed under a microscope.

2. The formulated products of example 1, example 2 and example 3 and the formulated products of comparative example 1 and example 2 were placed in a constant temperature and humidity cabinet: and (3) observing the product properties and observing the particle size under a microscope after standing for 3 months at the temperature of 30 +/-2 ℃ and the relative humidity of 60% +/-5%:

(1) Example 1 formulated product with no change in properties: oily and fine (as shown in fig. 6); the particle size is generally 1 μm and 2-4 μm larger when observed under a microscope;

(2) Example 2 formulated product with no change in properties: oily and fine (as shown in fig. 7); the particle size is generally 1 μm, compared with 2-3 μm when observed under a microscope;

(3) Example 3 formulated product with no change in properties: oily and fine (as shown in fig. 8); the particle size is generally 1 μm and larger is 2-3 μm when observed under a microscope;

(4) Comparative example 1 preparation of product properties: the paste appearance is completely layered, and the coarse feeling is obvious (as shown in figure 9); the particle size is 40-50 μm and larger is 55-60 μm when observed under a microscope;

(5) Comparative example 2 preparation of product properties: the appearance of the paste is completely layered, and the fineness is slightly changed (as shown in figure 10); the particle size is typically 5-7 μm, larger 8-10 μm, when observed under a microscope.

And (4) conclusion: as can be seen from the experimental examples, the prepared products in the examples 1, 2 and 3 are oily and fine, and the particle size is smaller than that of the prepared product in the comparative example, so that the transdermal absorption is facilitated; after the dimeticone emulsifiable paste is placed in a constant-temperature and constant-humidity drying oven for 3 months, the demulsification change of separation of oil phase components and water phase components does not occur, and the particle size is not changed, which shows that the dimeticone emulsifiable paste prepared by the product formula provided by the invention through the method has stable quality and good properties.

The demulsification and stratification in the comparative example 1 may be caused by incomplete dissolution of sorbic acid, nonuniform mixing of substances and no homogenization for viscosity adjustment, so that the subsequently prepared product has larger particles and poorer properties and is easy to delaminate and demulsify after long-term storage.

In the invention, the carbomer is a pharmaceutical adjuvant carbomer B type.

The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims

1. A method for preparing dimeticone cream is characterized by comprising the following steps:

the raw materials for preparing the dimeticone cream comprise: 100 parts of dimethicone, 20 parts of white petrolatum, 5 parts of carbomer, 100 parts of polyoxyl (40) stearate, 1 part of sorbic acid, and 274 parts of purified water;

the preparation method of the simethicone cream comprises the following steps:

b. mixing and stirring 100 parts of dimethicone, 20 parts of white vaseline and carbomer transparent gel uniformly to obtain a pre-emulsified gel system;

c. adding 1 part of sorbic acid and 224 parts of purified water into 100 parts of polyoxyl (40) stearate, and heating to 100-120 ℃ to dissolve to obtain a water phase;

d. adding the water phase into the pre-emulsified gel system, and uniformly stirring to obtain a secondary emulsified paste body;

e. grinding the secondary emulsified paste body in a colloid mill to obtain the simethicone coarse cream;

2. The method of claim 1, wherein the simethicone cream comprises: the viscosity of the dimeticone is 1000cs-1500cs.

3. The method of claim 2, wherein the simethicone cream comprises: in the step f, the homogenization time is 10-20 minutes, so that the dimethicone cream with reduced viscosity is obtained.

4. The method of claim 3, wherein the simethicone cream comprises: the grinding time in the step e is 0.5-1 hour.

5. The method of claim 4, wherein the simethicone cream comprises: and b, mixing and stirring in the step b at the speed of 600 revolutions per minute for 0.5 to 1 hour.

6. The method of claim 5, wherein the simethicone cream comprises: the step a specifically comprises the following steps: slowly and uniformly adding 5 parts of carbomer into 50 parts of purified water, stirring, putting into a refrigerator, freezing, taking out and stirring once every 6min, wherein the freezing temperature is-20 ℃, and freezing for 30min to obtain carbomer transparent gel.