CN111437246B - Preparation method for improving stability of cream product - Google Patents
Preparation method for improving stability of cream product Download PDFInfo
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- CN111437246B CN111437246B CN202010366718.8A CN202010366718A CN111437246B CN 111437246 B CN111437246 B CN 111437246B CN 202010366718 A CN202010366718 A CN 202010366718A CN 111437246 B CN111437246 B CN 111437246B
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- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/06—Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
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- A61K31/17—Amides, e.g. hydroxamic acids having the group >N—C(O)—N< or >N—C(S)—N<, e.g. urea, thiourea, carmustine
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
- A61K31/353—3,4-Dihydrobenzopyrans, e.g. chroman, catechin
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- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
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Abstract
The invention discloses a preparation method for improving the stability of a cream product, which comprises the following steps: A. preparing an oil phase; B. preparing a water phase; C. mixing the two phases: preheating a main pot to 50 ℃, adding the oil phase into the main pot, starting to stir at the speed of 10r/min, adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing to stir while starting an emulsifying function, and carrying out heat preservation, emulsification and stirring at the speed of 3300 r/min for 18-30 minutes; D. pretreating the main medicine; E. mixing and emulsifying: cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot; then starting an emulsification function, and carrying out heat preservation emulsification at the speed of 3300 r/min for 36-50 minutes; F. cooling to obtain cream. The preparation method of the invention obviously improves the emulsification effect of the cream product, and effectively solves the oil-water separation phenomenon of the urea vitamin E cream, thereby improving the stability of the product.
Description
Technical Field
The invention relates to the technical field of pharmacy, in particular to a preparation method for improving the stability of a cream product.
Background
The semisolid external preparation with certain consistency prepared by uniformly mixing the medicament and a proper matrix is ointment, and the ointment prepared by using the emulsion matrix is called cream, and mainly has the functions of protecting a wound surface, lubricating skin and locally treating. The general preparation method of the cream comprises the following steps: heating the oil phase and the water phase to a certain temperature respectively, mixing the two phases at constant temperature, adding the main drug, emulsifying, stirring, and cooling to obtain paste.
Cream products currently produced include: triamcinolone acetonide econazole cream, miconazole clobetasol cream, triamcinolone acetonide cream, acyclovir cream, miconazole nitrate cream, vefenamate vee cream, phentermine cream, ketoconazole cream, compound lactic acid cream, bifonazole cream, and urea vee cream.
However, the cream products used at present and the cream products prepared by the existing preparation methods still have the following problems:
the existing cream product has the defects of poor stability, oil-water separation, main medicine precipitation and the like after being stored for a period of time, and the effective period of the product is short.
Disclosure of Invention
Based on the above situation, the present invention aims to provide a preparation method for improving the stability of cream products, which can effectively solve the above problems. According to the preparation method for improving the stability of the cream product, the process steps are adjusted, two-time (two-step) emulsification is adopted and the emulsification time is prolonged, so that the emulsification effect of the cream product is obviously improved, the emulsification is increased when two phases are mixed and main drugs are mixed respectively, the oil-water separation phenomenon of the urea vitamin E cream can be solved, and the stability of the product is improved.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for preparing a cream product with improved stability comprises the following steps:
A. preparing an oil phase:
adding the weighed hexadecanol, octadecanol, white vaseline and ethylparaben into an oil phase pot, and heating and melting at 75-85 ℃; after melting, adding weighed vitamin E for dissolving, heating and melting, and then stirring for 5 minutes at the temperature of 75-85 ℃ to obtain an oil phase;
B. preparation of an aqueous phase:
adding weighed glycerol, propylene glycol, sodium dodecyl sulfate and 5/6-7/8 purified water into a water phase pot, and heating to 75-85 ℃ for dissolving; after dissolution, stirring for 5 minutes under heat preservation to obtain a water phase;
C. mixing the two phases:
preheating a main pot to 50 ℃, adding the oil phase into the main pot, starting to stir at the speed of 10r/min, adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing to stir while starting an emulsifying function, and carrying out heat preservation, emulsification and stirring at the speed of 3300 r/min for 18-30 minutes;
D. main medicine pretreatment:
putting the weighed rest purified water into a water phase pot (the same as the step A or the other port), adding urea, stirring and dissolving until the urea is completely dissolved;
E. mixing and emulsifying:
cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot; then starting an emulsification function, and carrying out heat preservation emulsification at the speed of 3300 r/min for 36-50 minutes;
F. cooling to form paste:
stirring at a speed of 10r/min, and cooling to below 35 deg.C to obtain the cream product.
Preferably, the cream product is a urea vitamin E cream.
Preferably, the cream product is prepared from the following raw materials in parts by weight:
145-155 parts of urea, 9.6-10.4 parts of vitamin E, 38-42 parts of hexadecanol, 43-47 parts of octadecanol, 72-78 parts of white vaseline, 0.95-1.05 parts of ethylparaben, 72-77 parts of glycerol, 74-78 parts of propylene glycol, 14.5-15.5 parts of sodium dodecyl sulfate, 0.95-1.05 parts of rose essence and 495-530 parts of purified water.
Preferably, the cream product is prepared from the following raw materials in parts by weight:
150 parts of urea, 10 parts of vitamin E, 40 parts of hexadecanol, 45 parts of octadecanol, 75 parts of white vaseline, 1 part of ethylparaben, 75 parts of glycerol, 75 parts of propylene glycol, 15 parts of sodium dodecyl sulfate, 1 part of rose essence and 513 parts of purified water.
One of the main reasons for instability of the product is poor emulsification effect, and the other reason is that the formula has the problems of poor compatibility and difficult uniform emulsification and dispersion (but the formula cannot be easily adjusted to ensure the drug effect of the cream product).
Preferably, in step C, the two phases are mixed: preheating a main pot to 50 ℃, adding the oil phase into the main pot, starting to stir at the speed of 10r/min, adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing stirring while starting an emulsifying function, and carrying out heat preservation, emulsification and stirring at the speed of 3300 r/min for 20 minutes.
Preferably, in step E, the mixing and emulsifying: cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot; then starting the emulsification function, and carrying out heat preservation emulsification at the speed of 3300 r/min for 40 minutes.
Preferably, the aqueous phase pans used in step B and step D are different aqueous phase pans.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the preparation method for improving the stability of the cream product adopts twice emulsification through product process improvement, strictly controls the process condition parameters of each step (the control of the process condition parameters and the matching of the emulsification steps are the key for obtaining good emulsification effect, and can ensure good emulsification effect, especially adjust the emulsification parameters, only if the process condition parameters are controlled in a proper range), improves the emulsification effect of the product, greatly improves the stability of the cream product, and ensures the good stability of the product.
The preparation method for improving the stability of the cream product of the invention adopts two-time (two-step) emulsification and increases the emulsification time by adjusting the process steps, obviously improves the emulsification effect of the cream product, increases the emulsification when the two phases are mixed with the main drug respectively, can solve the oil-water separation phenomenon of the urea vitamin E cream, thereby improving the stability of the product.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the following description of the preferred embodiments of the present invention is provided in connection with specific examples, which should not be construed as limiting the present patent.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are conventionally obtained commercially or prepared by conventional methods.
A method for preparing a cream product with improved stability comprises the following steps:
A. preparing an oil phase:
adding the weighed hexadecanol, octadecanol, white vaseline and ethylparaben into an oil phase pot, and heating and melting at 75-85 ℃; after melting, adding weighed vitamin E for dissolving, heating and melting, and then stirring for 5 minutes at the temperature of 75-85 ℃ to obtain an oil phase;
B. preparing a water phase:
adding weighed glycerol, propylene glycol, sodium dodecyl sulfate and 5/6-7/8 purified water into a water phase pot, and heating to 75-85 ℃ for dissolving; after dissolution, stirring for 5 minutes under the condition of heat preservation to obtain a water phase;
C. mixing the two phases:
preheating a main pot to 50 ℃, adding the oil phase into the main pot, starting to stir at the speed of 10r/min, adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing to stir while starting an emulsifying function, and carrying out heat preservation, emulsification and stirring at the speed of 3300 r/min for 18-30 minutes;
D. main medicine pretreatment:
putting the weighed residual purified water into a water phase pot, adding urea, stirring and dissolving until the urea is completely dissolved;
E. mixing and emulsifying:
cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot; then starting an emulsification function, and carrying out heat preservation emulsification at the speed of 3300 r/min for 36-50 minutes;
F. cooling to form paste:
stirring at a speed of 10r/min, and cooling to below 35 deg.C to obtain the cream product.
Preferably, the cream product is a urea vitamin E cream.
Preferably, the cream product is prepared from the following raw materials in parts by weight:
145-155 parts of urea, 9.6-10.4 parts of vitamin E, 38-42 parts of hexadecanol, 43-47 parts of octadecanol, 72-78 parts of white vaseline, 0.95-1.05 parts of ethylparaben, 72-77 parts of glycerol, 74-78 parts of propylene glycol, 14.5-15.5 parts of sodium dodecyl sulfate, 0.95-1.05 parts of rose essence and 495-530 parts of purified water.
Preferably, the cream product is prepared from the following raw materials in parts by weight:
150 parts of urea, 10 parts of vitamin E, 40 parts of hexadecanol, 45 parts of octadecanol, 75 parts of white vaseline, 1 part of ethylparaben, 75 parts of glycerol, 75 parts of propylene glycol, 15 parts of sodium dodecyl sulfate, 1 part of rose essence and 513 parts of purified water.
Preferably, in step C, the two phases are mixed: preheating a main pot to 50 ℃, adding the oil phase into the main pot, starting to stir at the speed of 10r/min, adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing to stir while starting the emulsifying function, and carrying out heat preservation, emulsification and stirring at the speed of 3300 r/min for 20 minutes.
Preferably, in step E, the mixing and emulsifying: cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot; then starting the emulsification function, and carrying out heat preservation and emulsification for 40 minutes at the speed of 3300 revolutions per minute.
Preferably, the aqueous phase pans used in step B and step D are different aqueous phase pans.
Example 1:
the raw materials comprise: 150g of urea, 10g g of vitamin E, 40g of hexadecanol, 45g of octadecanol, 75g of white vaseline, 1g of ethylparaben, 75g of glycerol, 75g of propylene glycol, 15g of sodium dodecyl sulfate, 1g of rose essence and 513g of purified water to prepare 1000g of urea vitamin E cream.
The preparation process comprises the following steps:
preparing an oil phase: adding the weighed hexadecanol, octadecanol, white vaseline and ethylparaben into an oil phase pot, and heating and melting at 75-85 ℃; after melting, adding weighed vitamin E for dissolving, heating and melting, and then keeping the temperature at 75-85 ℃ and stirring for 5 minutes.
Preparation of an aqueous phase: adding the weighed glycerol, propylene glycol, sodium dodecyl sulfate and purified water (reserved main drug dissolving water) into a water phase pot, and heating and dissolving at 75-85 ℃. Stirring for 5 minutes under heat preservation, and preserving heat for later use.
Mixing the two phases: preheating the main pot to 50 ℃, adding the oil phase into the main pot, starting stirring (10 r/min), adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing stirring while starting an emulsifying function (3300 r/min), preserving heat, emulsifying and stirring for 20 minutes.
Main drug pretreatment (dissolution): and (3) putting the weighed purified water into a water phase pot, adding urea, and stirring for dissolving.
Mixing and emulsifying: cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot. Starting an emulsification function (3300 r/min), and carrying out heat preservation and emulsification for 40 minutes.
Cooling to form paste: the temperature was reduced to below 35 ℃ with stirring (10 r/min) and the cream was visually observed to have formed.
A plurality of prepared emulsifiable paste is taken and put into a colorimetric tube of 25ml, each tube of emulsifiable paste is put into two thirds of the colorimetric tube, and 9 tubes are totally put. The mouth of pipe is sealed firmly with the sealing film, and the serial number is numbered, and 1 ~ 3 colour comparison tube is placed in refrigerator freezer, and 4 ~ 6 colour comparison tube is placed in the acceleration test case of 40 + -2 ℃, and 7 ~ 9 colour comparison tube room temperature is deposited. And taking out the colorimetric tubes in the freezing chamber and the acceleration test box of the refrigerator after 24 hours, placing the colorimetric tubes to room temperature, observing the characters of the emulsifiable paste in the colorimetric tubes, wherein the emulsifiable paste in the No. 1-6 colorimetric tubes is not layered and has no difference compared with No. 7-9.
Example 2:
the raw materials comprise: 150g of urea, 10g g of vitamin E, 40g of hexadecanol, 45g of octadecanol, 75g of white vaseline, 1g of ethylparaben, 75g of glycerol, 75g of propylene glycol, 15g of sodium dodecyl sulfate, 1g of rose essence and 513g of purified water to prepare 1000g of urea vitamin E cream.
The preparation process comprises the following steps:
preparing an oil phase: adding the weighed hexadecanol, octadecanol, white vaseline and ethylparaben into an oil phase pot, and heating and melting at 75-85 ℃; after melting, adding weighed vitamin E for dissolving, heating and melting, and then keeping the temperature at 75-85 ℃ and stirring for 5 minutes.
Preparation of an aqueous phase: adding the weighed glycerol, propylene glycol, sodium dodecyl sulfate and purified water (reserved main drug dissolving water) into a water phase pot, and heating and dissolving at 75-85 ℃. Stirring for 5 minutes under heat preservation, and preserving heat for later use.
Mixing the two phases: preheating the main pot to 50 ℃, adding the oil phase into the main pot, starting stirring (10 r/min), adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing stirring while starting an emulsifying function (3300 r/min), preserving heat, emulsifying and stirring for 30 minutes.
Main drug pretreatment (dissolution): and (3) putting the weighed purified water into a water phase pot, adding urea, and stirring for dissolving.
Mixing and emulsifying: cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot. Starting an emulsification function (3300 r/min), and carrying out heat preservation and emulsification for 40 minutes.
Cooling to form paste: the temperature was reduced to below 35 ℃ with stirring (10 r/min) and the cream was visually observed to have formed.
A plurality of prepared emulsifiable paste is taken and put into a colorimetric tube of 25ml, each tube of emulsifiable paste is put into two thirds of the colorimetric tube, and 9 tubes are totally put. The mouth of pipe is sealed firmly with the sealing film, and the serial number is numbered, and 1 ~ 3 colour comparison tube is placed in refrigerator freezer, and 4 ~ 6 colour comparison tube is placed in the acceleration test case of 40 + -2 ℃, and 7 ~ 9 colour comparison tube room temperature is deposited. The color comparison tube in the refrigerator freezing chamber and the acceleration test box is taken out after 24 hours, the color comparison tube is placed at room temperature, the characters of the emulsifiable paste in the color comparison tube are observed, the emulsifiable paste in the No. 1-6 color comparison tube is not layered, and no difference exists compared with No. 7-9.
Example 3:
the raw materials comprise: 150g of urea, 10g g of vitamin E, 40g of hexadecanol, 45g of octadecanol, 75g of white vaseline, 1g of ethylparaben, 75g of glycerol, 75g of propylene glycol, 15g of sodium dodecyl sulfate, 1g of rose essence and 513g of purified water to prepare 1000g of urea vitamin E cream.
The preparation process comprises the following steps:
preparing an oil phase: adding the weighed hexadecanol, octadecanol, white vaseline and ethylparaben into an oil phase pot, and heating and melting at 75-85 ℃; after the melting, the weighed vitamin E is added for dissolving, and after the heating and melting, the heat preservation and the stirring are carried out for 5 minutes at the temperature of 75-85 ℃.
Preparation of an aqueous phase: adding the weighed glycerol, propylene glycol, sodium dodecyl sulfate and purified water (reserved main drug dissolving water) into a water phase pot, and heating and dissolving at 75-85 ℃. Stirring for 5 minutes under heat preservation, and preserving heat for later use.
Mixing the two phases: preheating the main pot to 50 ℃, adding the oil phase into the main pot, starting stirring (10 r/min), adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing stirring while starting an emulsifying function (3300 r/min), preserving heat, emulsifying and stirring for 20 minutes.
Main drug pretreatment (dissolution): and (3) putting the weighed purified water into a water phase pot, adding urea, and stirring for dissolving.
Mixing and emulsifying: cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot. Starting an emulsification function (3300 r/min), and carrying out heat preservation and emulsification for 50 minutes.
Cooling to form paste: the temperature was reduced to below 35 ℃ with stirring (10 r/min) and the cream was visually observed to have formed.
A plurality of prepared emulsifiable paste is taken and put into a colorimetric tube of 25ml, each tube of emulsifiable paste is put into two thirds of the colorimetric tube, and 9 tubes are totally put. The mouth of pipe is sealed firmly with the sealing film, and the serial number is numbered, and 1 ~ 3 colour comparison tube is placed in refrigerator freezer, and 4 ~ 6 colour comparison tube is placed in the acceleration test case of 40 + -2 ℃, and 7 ~ 9 colour comparison tube room temperature is deposited. And taking out the colorimetric tubes in the freezing chamber and the acceleration test box of the refrigerator after 24 hours, placing the colorimetric tubes to room temperature, observing the characters of the emulsifiable paste in the colorimetric tubes, wherein the emulsifiable paste in the No. 1-6 colorimetric tubes is not layered and has no difference compared with No. 7-9.
Comparative example 1:
the raw materials comprise: 150g of urea, 10g g of vitamin E, 40g of hexadecanol, 45g of octadecanol, 75g of white vaseline, 1g of ethylparaben, 75g of glycerol, 75g of propylene glycol, 15g of sodium dodecyl sulfate, 1g of rose essence and 513g of purified water to prepare 1000g of urea vitamin E cream.
The preparation process comprises the following steps:
preparing an oil phase: adding the weighed hexadecanol, octadecanol, white vaseline and ethylparaben into an oil phase pot, and heating and melting at 75-85 ℃; after melting, adding weighed vitamin E for dissolving, heating and melting, and then keeping the temperature at 75-85 ℃ and stirring for 5 minutes.
Preparing a water phase: adding the weighed glycerol, propylene glycol, sodium dodecyl sulfate and purified water (reserved water for dissolving the main drugs) into a water phase pot, and heating and dissolving at 75-85 ℃. Stirring for 5 minutes under heat preservation, and preserving heat for later use.
Mixing the two phases: preheating the main pot to 50 ℃, adding the oil phase into the main pot, starting stirring (10 r/min), adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing stirring while starting an emulsifying function (3300 r/min), preserving heat, emulsifying and stirring for 10 minutes.
Main drug pretreatment (dissolution): and putting the weighed purified water into a water phase pot, adding urea, and stirring for dissolving.
Mixing and emulsifying: cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot. Starting an emulsification function (3300 r/min), and carrying out heat preservation and emulsification for 40 minutes.
Cooling to form paste: the temperature was reduced to below 35 ℃ with stirring (10 r/min) and the cream was visually observed to have formed.
A plurality of prepared emulsifiable paste is taken and put into a colorimetric tube of 25ml, each tube of emulsifiable paste is put into two thirds of the colorimetric tube, and 9 tubes are totally put. The mouth of pipe is sealed firmly with the sealing film, and the serial number is numbered, and 1 ~ 3 colour comparison tube is placed in refrigerator freezer, and 4 ~ 6 colour comparison tube is placed in the acceleration test case of 40 + -2 ℃, and 7 ~ 9 colour comparison tube room temperature is deposited. And taking out the colorimetric tubes in the refrigerating chamber and the acceleration test box of the refrigerator after 24 hours, placing the colorimetric tubes to room temperature, observing the characters of the emulsifiable paste in the colorimetric tubes, wherein the emulsifiable paste in the No. 1-6 colorimetric tubes is not layered, is slightly thinner than that of No. 7-9 colorimetric tubes and has fluidity.
Comparative example 2:
the raw materials comprise: 150g of urea, 10g g of vitamin E, 40g of hexadecanol, 45g of octadecanol, 75g of white vaseline, 1g of ethylparaben, 75g of glycerol, 75g of propylene glycol, 15g of sodium dodecyl sulfate, 1g of rose essence and 513g of purified water to prepare 1000g of urea vitamin E cream.
The preparation process comprises the following steps:
preparing an oil phase: adding the weighed hexadecanol, octadecanol, white vaseline and ethylparaben into an oil phase pot, and heating and melting at 75-85 ℃; after melting, adding weighed vitamin E for dissolving, heating and melting, and then keeping the temperature at 75-85 ℃ and stirring for 5 minutes.
Preparing a water phase: adding the weighed glycerol, propylene glycol, sodium dodecyl sulfate and purified water (reserved water for dissolving the main drugs) into a water phase pot, and heating and dissolving at 75-85 ℃. Stirring for 5 minutes under heat preservation, and preserving heat for later use.
Mixing the two phases: preheating a main pot to 50 ℃, adding an oil phase into the main pot, starting stirring (10 r/min), adding a water phase into the main pot, mixing and stirring for 5 minutes, continuing stirring, starting an emulsifying function (3300 r/min), preserving heat, emulsifying and stirring for 20 minutes.
Main drug pretreatment (dissolution): and putting the weighed purified water into a water phase pot, adding urea, and stirring for dissolving.
Mixing and emulsifying: cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot. Starting an emulsification function (3300 revolutions per minute), and carrying out heat preservation and emulsification for 30 minutes.
Cooling to form paste: the temperature was reduced to below 35 ℃ with stirring (10 r/min) and the cream was visually observed to have formed.
A plurality of prepared emulsifiable paste is taken and put into a colorimetric tube of 25ml, each tube of emulsifiable paste is put into two thirds of the colorimetric tube, and 9 tubes are totally put. The mouth of pipe is sealed firmly with the sealing film, and the serial number is numbered, and 1 ~ 3 colour comparison tube is placed in refrigerator freezer, and 4 ~ 6 colour comparison tube is placed in the acceleration test case of 40 + -2 ℃, and 7 ~ 9 colour comparison tube room temperature is deposited. And taking out the colorimetric tubes in the refrigerating chamber and the acceleration test box of the refrigerator after 24 hours, placing the colorimetric tubes to room temperature, observing the characters of the emulsifiable paste in the colorimetric tubes, wherein the emulsifiable paste in the No. 1-6 colorimetric tubes is not layered, is slightly thinner than that of No. 7-9 colorimetric tubes and has fluidity.
Comparative example 3:
the raw materials comprise: 150g of urea, 10g g of vitamin E, 40g of hexadecanol, 45g of octadecanol, 75g of white vaseline, 1g of ethylparaben, 75g of glycerol, 75g of propylene glycol, 15g of sodium dodecyl sulfate, 1g of rose essence and 513g of purified water to prepare 1000g of urea vitamin E cream.
The preparation process comprises the following steps:
preparing an oil phase: adding the weighed hexadecanol, octadecanol, white vaseline and ethylparaben into an oil phase pot, and heating and melting at 75-85 ℃; after melting, adding weighed vitamin E for dissolving, heating and melting, and then keeping the temperature at 75-85 ℃ and stirring for 5 minutes.
Preparing a water phase: adding the weighed glycerol, propylene glycol, sodium dodecyl sulfate and purified water (reserved main drug dissolving water) into a water phase pot, and heating and dissolving at 75-85 ℃. Stirring for 5 minutes under heat preservation, and preserving heat for later use.
Mixing the two phases: preheating the main pot to 50 ℃, adding the oil phase into the main pot, starting stirring (10 r/min), adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing stirring while starting an emulsifying function (3300 r/min), preserving heat, emulsifying and stirring for 20 minutes.
Main drug pretreatment (dissolution): and (3) putting the weighed purified water into a water phase pot, adding urea, and stirring for dissolving.
Mixing and emulsifying: cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot. Starting an emulsification function (3300 r/min), and carrying out heat preservation and emulsification for 20 minutes.
Cooling to form paste: the temperature was reduced to below 35 ℃ with stirring (10 r/min) and the cream was visually observed to have formed.
A plurality of prepared emulsifiable paste is taken and put into a colorimetric tube of 25ml, each tube of emulsifiable paste is put into two thirds of the colorimetric tube, and 9 tubes are totally put. The mouth of the tube is firmly sealed by a sealing film, the tube is numbered, a No. 1 to No. 3 colorimetric tubes are placed in a refrigerator freezing chamber, a No. 4 to No. 6 colorimetric tubes are placed in an acceleration test box at 40 +/-2 ℃, and the No. 7 to No. 9 colorimetric tubes are stored at room temperature. Taking out the colorimetric tubes in the freezing chamber and the acceleration test box of the refrigerator after 24 hours, placing the colorimetric tubes to room temperature, observing the characters of the emulsifiable paste in the colorimetric tubes, wherein the emulsifiable paste in the No. 1-6 colorimetric tubes is not layered and is thinner than the emulsifiable paste in the No. 7-9 colorimetric tubes and is between a liquid state and a semisolid state.
Comparative example 4:
the raw materials comprise: 150g of urea, 10g g of vitamin E, 40g of hexadecanol, 45g of octadecanol, 75g of white vaseline, 1g of ethylparaben, 75g of glycerol, 75g of propylene glycol, 15g of sodium dodecyl sulfate, 1g of rose essence and 513g of purified water to prepare 1000g of urea vitamin E cream.
The preparation process comprises the following steps:
preparing an oil phase: adding the weighed hexadecanol, octadecanol, white vaseline and ethylparaben into an oil phase pot, and heating and melting at 75-85 ℃; after melting, adding weighed vitamin E for dissolving, heating and melting, and then keeping the temperature at 75-85 ℃ and stirring for 5 minutes.
Preparation of an aqueous phase: adding the weighed glycerol, propylene glycol, sodium dodecyl sulfate and purified water (reserved main drug dissolving water) into a water phase pot, and heating and dissolving at 75-85 ℃. Stirring for 5 minutes under heat preservation, and preserving heat for later use.
Mixing the two phases: preheating the main pot to 50 ℃, adding the oil phase into the main pot, starting stirring (10 r/min), adding the water phase into the main pot, and mixing and stirring for 5 minutes.
Main drug pretreatment (dissolution): and putting the weighed purified water into a water phase pot, adding urea, and stirring for dissolving.
Mixing and emulsifying: cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot. Starting an emulsification function (3300 r/min), and carrying out heat preservation and emulsification for 40 minutes.
Cooling to form paste: the temperature was reduced to below 35 ℃ with stirring (10 r/min) and the cream was visually observed to have formed.
A plurality of prepared emulsifiable paste is taken and put into a colorimetric tube of 25ml, each tube of emulsifiable paste is put into two thirds of the colorimetric tube, and 9 tubes are totally put. The mouth of pipe is sealed firmly with the sealing film, and the serial number is numbered, and 1 ~ 3 colour comparison tube is placed in refrigerator freezer, and 4 ~ 6 colour comparison tube is placed in the acceleration test case of 40 + -2 ℃, and 7 ~ 9 colour comparison tube room temperature is deposited. Taking out the colorimetric tubes in the freezing chamber and the acceleration test box of the refrigerator after 24 hours, placing the colorimetric tubes to room temperature, observing the characters of the emulsifiable paste in the colorimetric tubes, wherein the emulsifiable paste in the No. 1-6 colorimetric tubes is not layered and is thinner than the emulsifiable paste in the No. 7-9 colorimetric tubes and is between a liquid state and a semisolid state.
Comparative example 5:
the raw materials comprise: 150g of urea, 10g g of vitamin E, 40g of hexadecanol, 45g of octadecanol, 75g of white vaseline, 1g of ethylparaben, 75g of glycerol, 75g of propylene glycol, 15g of sodium dodecyl sulfate, 1g of rose essence and 513g of purified water to prepare 1000g of urea vitamin E cream.
The preparation process comprises the following steps:
preparing an oil phase: adding the weighed hexadecanol, octadecanol, white vaseline and ethylparaben into an oil phase pot, and heating and melting at 75-85 ℃; after the melting, the weighed vitamin E is added for dissolving, and after the heating and melting, the heat preservation and the stirring are carried out for 5 minutes at the temperature of 75-85 ℃.
Preparation of an aqueous phase: adding the weighed glycerol, propylene glycol, sodium dodecyl sulfate and purified water (reserved water for dissolving the main drugs) into a water phase pot, and heating and dissolving at 75-85 ℃. Stirring for 5 minutes under heat preservation, and preserving heat for later use.
Mixing the two phases: preheating the main pot to 50 ℃, adding the oil phase into the main pot, stirring (10 r/min), adding the water phase into the main pot, mixing and stirring for 5 minutes.
Main drug pretreatment (dissolution): and putting the weighed purified water into a water phase pot, adding urea, and stirring for dissolving.
Mixing and emulsifying: cooling the main pot, and adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃. Then adding the rose essence into the main pot. Starting an emulsification function (3300 revolutions per minute), and carrying out heat preservation and emulsification for 20 minutes.
Cooling to form paste: the temperature was reduced to below 35 ℃ with stirring (10 r/min) and the cream was visually observed to have formed.
A plurality of prepared emulsifiable paste is taken and put into a colorimetric cylinder of 25ml, each tube of emulsifiable paste is put into two thirds of the colorimetric cylinder, and 9 tubes are arranged in total. The mouth of pipe is sealed firmly with the sealing film, and the serial number is numbered, and 1 ~ 3 colour comparison tube is placed in refrigerator freezer, and 4 ~ 6 colour comparison tube is placed in the acceleration test case of 40 + -2 ℃, and 7 ~ 9 colour comparison tube room temperature is deposited. Taking out the colorimetric tubes in the refrigerator freezing chamber and the acceleration test box after 24 hours, putting the colorimetric tubes to room temperature, observing the characters of the emulsifiable paste in the colorimetric tubes, and obviously layering and oil-water separation phenomena all appear in the emulsifiable paste in No. 1-6 colorimetric tubes.
The test results from the above examples and comparative examples show that: the emulsification is carried out twice (two steps) and the emulsification time is prolonged, so that the emulsification effect of the cream product is obviously improved, and the emulsification is respectively increased after the two phases are mixed and when the main drug is mixed, so that the oil-water separation phenomenon of the urea vitamin E cream can be effectively solved.
The above are only preferred embodiments of the present invention, and it should be noted that the above preferred embodiments should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (4)
1. The preparation method for improving the stability of the cream product is characterized in that the cream product is urea vitamin E cream, and the cream product is prepared from the following raw materials in parts by weight: 145-155 parts of urea, 9.6-10.4 parts of vitamin E, 38-42 parts of hexadecanol, 43-47 parts of octadecanol, 72-78 parts of white vaseline, 0.95-1.05 parts of ethylparaben, 72-77 parts of glycerol, 74-78 parts of propylene glycol, 14.5-15.5 parts of sodium dodecyl sulfate, 0.95-1.05 parts of rose essence and 495-530 parts of purified water; the preparation method comprises the following steps:
A. preparing an oil phase:
adding the weighed hexadecanol, octadecanol, white vaseline and ethylparaben into an oil phase pot, and heating and melting at 75-85 ℃; after melting, adding weighed vitamin E for dissolving, heating and melting, and then stirring for 5 minutes at the temperature of 75-85 ℃ to obtain an oil phase;
B. preparation of an aqueous phase:
adding weighed glycerol, propylene glycol, sodium dodecyl sulfate and 5/6-7/8 purified water into a water phase pot, and heating to 75-85 ℃ for dissolving; after dissolution, stirring for 5 minutes under heat preservation to obtain a water phase;
C. mixing the two phases:
preheating a main pot to 50 ℃, adding the oil phase into the main pot, starting to stir at the speed of 10r/min, adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing to stir while starting an emulsifying function, and carrying out heat preservation, emulsification and stirring at the speed of 3300 r/min for 18-30 minutes;
D. main medicine pretreatment:
putting the weighed residual purified water into a water phase pot, adding urea, stirring and dissolving until the urea is completely dissolved;
E. mixing and emulsifying:
cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot; then starting an emulsification function, and carrying out heat preservation emulsification at the speed of 3300 r/min for 36-50 minutes;
F. cooling to form paste:
stirring at a speed of 10r/min and cooling to below 35 ℃ to obtain the cream product;
the water phase pots used in the step B and the step D are different water phase pots.
2. The preparation method for improving the stability of the cream product according to claim 1, wherein the cream product is prepared from the following raw materials in parts by weight:
150 parts of urea, 10 parts of vitamin E, 40 parts of hexadecanol, 45 parts of octadecanol, 75 parts of white vaseline, 1 part of ethylparaben, 75 parts of glycerol, 75 parts of propylene glycol, 15 parts of sodium dodecyl sulfate, 1 part of rose essence and 513 parts of purified water.
3. The method of claim 1, wherein in step C, the two phases are mixed: preheating a main pot to 50 ℃, adding the oil phase into the main pot, starting to stir at the speed of 10r/min, adding the water phase into the main pot, mixing and stirring for 5 minutes, continuing stirring while starting an emulsifying function, and carrying out heat preservation, emulsification and stirring at the speed of 3300 r/min for 20 minutes.
4. The method of claim 3, wherein step E, mixing and emulsifying: cooling the main pot, adding the pretreated main medicine into the main pot when the temperature is reduced to 65-70 ℃, and then adding the rose essence into the main pot; then starting the emulsification function, and carrying out heat preservation emulsification at the speed of 3300 r/min for 40 minutes.
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