CN114469856B - Sodium usnate solution and preparation method thereof - Google Patents
Sodium usnate solution and preparation method thereof Download PDFInfo
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- CN114469856B CN114469856B CN202210068127.1A CN202210068127A CN114469856B CN 114469856 B CN114469856 B CN 114469856B CN 202210068127 A CN202210068127 A CN 202210068127A CN 114469856 B CN114469856 B CN 114469856B
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- sodium usnate
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- 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
- A61K31/34—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having five-membered rings with one oxygen as the only ring hetero atom, e.g. isosorbide
- A61K31/343—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having five-membered rings with one oxygen as the only ring hetero atom, e.g. isosorbide condensed with a carbocyclic ring, e.g. coumaran, bufuralol, befunolol, clobenfurol, amiodarone
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- 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
- A61K47/10—Alcohols; Phenols; Salts thereof, e.g. glycerol; Polyethylene glycols [PEG]; Poloxamers; PEG/POE alkyl ethers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/44—Oils, fats or waxes according to two or more groups of A61K47/02-A61K47/42; Natural or modified natural oils, fats or waxes, e.g. castor oil, polyethoxylated castor oil, montan wax, lignite, shellac, rosin, beeswax or lanolin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/08—Solutions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
Abstract
The application relates to a sodium usnate solution and a preparation method thereof, which are sequentially carried out according to the following steps: (1) Mixing sodium usnate, PEG 60-hydrogenated castor oil, glycerol and/or propylene glycol uniformly; (2) adding purified water to constant volume; and (3) stirring until all materials are dissolved. The sodium usnate extracting solution and the preparation method thereof provided by the invention overcome the problem of low content of sodium usnate caused by low solubility of sodium usnate in the conventional sodium usnate aqueous solution, and simultaneously solve the problems of more auxiliary materials, complex preparation process, non-clarified suspension and the like in the prior art for preparing the sodium usnate solution; the preparation method of the sodium usnate solution provided by the invention is simple in process, and the used auxiliary materials are few in types. The prepared solution is clear and bright, and the precipitation phenomenon can not occur after long-time low-temperature storage.
Description
Technical Field
The invention mainly relates to the technical field of medicines, in particular to a sodium usnate solution and a preparation method thereof.
The background art comprises the following steps:
usnic Acid (UA), also known as Usnic Acid, is derived from the dried lichen bodies of Usnea diflorata vain, and Usnea longissima ach, a plant of the family Usnea. The application fields of the sodium usnate and the sodium usnic acid are basically consistent, and the research contents at home and abroad mostly concentrate on the aspects of extraction and separation, biosynthesis, pharmacological activity and the like of the usnic acid. Usnic acid has the functions of resisting bacteria, radiation, corrosion and the like, is applied to industries such as dietary additives, perfume, cosmetics and the like, and is added into toothpaste, mouthwash, deodorant, sun oil, weight-losing products and the like as a pure substance. However, in the medical field, the research is still in progress, and only a few reports on the research of preparation products exist.
Usnic acid is a poorly soluble compound, and the solubility in water is lower than 0.1mg/mL, which greatly influences the application of usnic acid in clinic and the development of new drugs. From a large number of literatures about pharmacological activity research, it is presumed that usnic acid has certain membrane permeability after being dissolved by various methods, can enter bacteria and cells to play corresponding roles, and therefore, from the viewpoint of a biopharmaceutical classification system, usnic acid may be a class II drug, namely, has the characteristics of low solubility and high permeability. For such drugs, improved solubility is critical to improving bioavailability.
Therefore, the invention is especially provided.
Disclosure of Invention
The invention aims to provide a sodium usnate solution and a preparation method thereof, which solve the problems of low content of sodium usnate in the conventional sodium usnate solution and unstable system.
In order to realize the aim, the invention provides a preparation method of a sodium usnate solution, which comprises the following steps in sequence:
(1) Mixing sodium usnate, PEG 60-hydrogenated castor oil, glycerol and/or propylene glycol uniformly;
(2) Adding purified water to constant volume;
(3) Stirring until the materials are dissolved.
Preferably or optionally, the addition amount of the sodium usnate in the step (1) is 0.5-2g/100mL, the addition amount of the PEG 60-hydrogenated castor oil is 15-30g/100mL, and the addition amount of the glycerol and/or the propylene glycol is 2-20g/100mL.
Since PEG 60-hydrogenated castor oil is a paste-like substance having extremely poor fluidity at normal temperature. As shown in FIG. 1, 50% PEG 60-hydrogenated castor oil was also poor in fluidity, and 40% PEG 60-hydrogenated castor oil was also high in viscosity. Thus, PEG 60-hydrogenated castor oil concentrations of no more than 30% were selected.
Preferably or alternatively, the weight ratio of PEG 60-hydrogenated castor oil to sodium usnate is not less than 15.
Preferably or alternatively, the weight ratio of the glycerol and/or propylene glycol to the sodium usnate is not less than 2.
Preferably or optionally, the stirring step in step (3) is preceded by a heating step.
Preferably or alternatively, the temperature of the heating is 90-95 ℃.
Preferably or alternatively, the stirring step in the step (3) is heat-preservation stirring, and the heat-preservation temperature is 90-95 ℃.
Preferably or alternatively, the time for keeping warm and stirring in the step (3) is 10-20min.
The mode of heating, heat preservation and stirring is adopted, so that the dissolution of all materials can be accelerated, and the production efficiency is improved. It should be noted, however, that this step is not essential and the above materials may be dissolved by stirring at normal temperature.
On the other hand, the invention also provides a sodium usnate solution which is prepared by adopting the preparation method of the sodium usnate solution.
The sodium usnate solution and the preparation method thereof provided by the invention have the following advantages:
the problem of low content of sodium usnate caused by low solubility of sodium usnate in the conventional sodium usnate aqueous solution is solved, and the problems of more auxiliary materials, complex preparation process, non-clarification of suspension and the like in the prior art in the preparation of the sodium usnate solution are solved; the preparation method of the sodium usnate solution provided by the invention is simple in process, and the used auxiliary materials are few in variety. The prepared solution is clear and bright, and the precipitation phenomenon can not occur after long-time low-temperature storage.
Description of the drawings:
FIG. 1 is a graph comparing the state of PEG 60-hydrogenated castor oil at different concentrations;
FIG. 2 is a diagram showing a sample to which Tween 80 was added in example 1;
FIG. 3 is a diagram of a sample to which PEG200 was added in example 1;
FIG. 4 is a graph showing a sample to which glacial acetic acid was added in example 1;
FIG. 5 is a graph of a sample with the addition of OP-10 in example 1;
FIG. 6 is a graph of a sample of example 1 with ethanol added;
FIG. 7 is a graph of a sample of example 1 with the addition of PEG 60-hydrogenated castor oil;
FIG. 8 is a graph of a sample of example 1 with the addition of PEG 40-hydrogenated castor oil;
FIG. 9 is a graph of a sample of example 2 with the addition of PEG 40-hydrogenated castor oil;
FIG. 10 is a graph of a sample of example 2 with the addition of PEG 60-hydrogenated castor oil;
FIG. 11 is a diagram of a sample to which PEG200 was added in example 3;
FIG. 12 is a graph of a sample of example 3 with propylene glycol added;
FIG. 13 is a graph showing a sample of example 3 in which glycerol was added;
FIG. 14 is a graph comparing the stability after low temperature storage of samples 1-6 of example 4;
FIG. 15 is a graph comparing the stability after low temperature storage of samples 7-12 from example 4;
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
Example 1
Weighing 1g of usnic acid sodium in multiple parts, respectively adding 30g of tween 80, PEG200, glacial acetic acid, OP-10, ethanol, PEG 60-hydrogenated castor oil or PEG 40-hydrogenated castor oil, then using purified water to fix the volume to 100mL, and magnetically stirring for 60min.
As shown in FIGS. 2 to 8, the samples prepared by adding Tween 80, PEG200, glacial acetic acid, OP-10 and ethanol can not be clarified, while the samples prepared by adding PEG 60-hydrogenated castor oil and PEG 40-hydrogenated castor oil have better clarity.
Example 2
Weighing 2 parts of 1g of sodium usnate, adding 30g of PEG 60-hydrogenated castor oil or 30g of PEG 40-hydrogenated castor oil respectively, adding purified water to the mixture until the volume is 100mL, and magnetically stirring the mixture for 60min.
Each prepared sample was placed in a refrigerator at 4 ℃ for continuous observation.
As shown in FIGS. 9 to 10, the sample with the addition of PEG 40-hydrogenated castor oil precipitated the next day, and the sample with the addition of PEG 60-hydrogenated castor oil precipitated a little at day 12.
Example 3
3 parts of 1g of usnic acid sodium is weighed, 30g of PEG 60-hydrogenated castor oil is added into each part, 20g of propylene glycol, glycerol or PEG200 is added respectively, purified water is used for fixing the volume to 100mL respectively, and then magnetic stirring is carried out for 60min.
Each prepared sample was placed in a refrigerator at 4 ℃ for continuous observation.
As shown in FIGS. 11 to 13, the samples to which PEG200 was added began to precipitate slightly on day 15, while the samples to which propylene glycol or glycerin was added did not precipitate even on day 60.
Example 4
12 parts of 1g of sodium usnate is weighed, PEG 60-hydrogenated castor oil and glycerol are added into each part of sodium usnate according to the table 1, then each sample is respectively added with purified water to be 100mL, and the mixture is magnetically stirred for 60min.
Each prepared sample was placed in a refrigerator at 4 ℃ for continuous observation.
TABLE 1 different dosages PEG 60-hydrogenated Castor oil and Glycerol design Table (g)
As shown in FIGS. 14 to 15, samples 1 to 12 in this example correspond to samples Nos. 11 to 22 in FIGS. 14 and 15, respectively. As can be seen from the figure, for the sodium usnate solution with the concentration of 1g/100mL, the PEG 60-hydrogenated castor oil with the concentration of not less than 15g/100mL is matched with the glycerol with the concentration of not less than 2g/100mL, so that the prepared sodium usnate solution can be ensured not to be separated out in the process of storing at the low temperature of 4 ℃ for 60 days.
Example 5
The sodium usnate solution is prepared according to the following proportion and flow.
Sample No. 13: weighing 1g of usnic acid sodium; PEG 60-hydrogenated castor oil 30; 12g of glycerol; the volume of the purified water is 100mL, the purified water is heated to 95 ℃, and the purified water is stirred for 12min under the condition of heat preservation.
Sample 14: weighing 0.5g of usnic acid sodium; 15g of PEG 60-hydrogenated castor oil; 2g of glycerol; the volume of the purified water is 100mL, the purified water is heated to 90 ℃, and the purified water is stirred for 15min under the condition of heat preservation.
Sample 15: weighing 0.8g of usnic acid sodium; 30g of PEG 60-hydrogenated castor oil; 14g of glycerol; the volume of the purified water is 100mL, the purified water is heated to 95 ℃, and the purified water is stirred for 15min under the condition of heat preservation.
Sample 16: weighing 1g of usnic acid sodium; 20g of PEG 60-hydrogenated castor oil; 15g of glycerol; the volume of the purified water is 100mL, the purified water is heated to 95 ℃, and the purified water is stirred for 20min under the condition of heat preservation.
Sample 17: weighing 2g of usnic acid sodium; 30g of PEG 60-hydrogenated castor oil; 20g of glycerol; the volume of the purified water is 100mL, the purified water is heated to 95 ℃, and the purified water is stirred for 20min under the condition of heat preservation.
Sample 18: weighing 1g of usnic acid sodium; 30g of PEG 60-hydrogenated castor oil; 16g of glycerol; the volume of the purified water is 100mL, the purified water is heated to 93 ℃, and the purified water is stirred for 15min under the condition of heat preservation.
Sample 19: weighing 2g of usnic acid sodium; 30g of PEG 60-hydrogenated castor oil; 20g of propylene glycol; the volume of the purified water is 100mL, the purified water is heated to 95 ℃, and the purified water is stirred for 20min under the condition of heat preservation.
Sample 20: weighing 0.5g of usnic acid sodium; 15g of PEG 60-hydrogenated castor oil; 2g of propylene glycol; and (4) adding purified water to 100mL, heating to 90 ℃, and keeping the temperature and stirring for 15min.
No precipitation phenomenon occurs in the process of storing samples 13-20 at the low temperature of 4 ℃ for 60 days, and the samples are clear and bright. The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are all within the protection scope of the present invention.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (6)
1. A preparation method of a sodium usnate solution is characterized by comprising the following steps in sequence:
(1) Mixing sodium usnate, PEG 60-hydrogenated castor oil, glycerol and/or propylene glycol uniformly; wherein the addition amount of the sodium usnate is 0.5-2g/100mL, the addition amount of the PEG 60-hydrogenated castor oil is 15-30g/100mL, the addition amount of the glycerol and/or the propylene glycol is 2-20g/100mL, the weight ratio of the PEG 60-hydrogenated castor oil to the sodium usnate is not less than 15, and the weight ratio of the glycerol and/or the propylene glycol to the sodium usnate is not less than 2;
(2) Adding purified water to constant volume;
(3) Stirring until the materials are dissolved.
2. The method for preparing a sodium usnate solution according to claim 1, wherein the stirring step in step (3) is preceded by a heating step.
3. The method for preparing sodium usnate solution according to claim 2, wherein the heating temperature is 90-95 ℃.
4. The method for preparing sodium usnate solution according to claim 2, wherein the stirring step in step (3) is performed while keeping the temperature at 90-95 ℃.
5. The method for preparing a sodium usnate solution according to claim 1, wherein the time for keeping warm and stirring in step (3) is 10-20min.
6. A sodium usnate solution characterized by being prepared by the method for producing a sodium usnate solution according to any one of claims 1 to 5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210068127.1A CN114469856B (en) | 2022-01-20 | 2022-01-20 | Sodium usnate solution and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210068127.1A CN114469856B (en) | 2022-01-20 | 2022-01-20 | Sodium usnate solution and preparation method thereof |
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| CN114469856B true CN114469856B (en) | 2023-01-31 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5417962A (en) * | 1992-01-24 | 1995-05-23 | The Gillette Company | Usnic acid deodorant stick |
| CN106943341A (en) * | 2017-05-10 | 2017-07-14 | 重庆理工大学 | A kind of external preparation for improving usnic acid Transdermal absorption and its application in skin wound healing is promoted |
| WO2017134594A1 (en) * | 2016-02-04 | 2017-08-10 | Apharm S.R.L. | New topical compositions comprising usnic acid and their use in therapy |
-
2022
- 2022-01-20 CN CN202210068127.1A patent/CN114469856B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5417962A (en) * | 1992-01-24 | 1995-05-23 | The Gillette Company | Usnic acid deodorant stick |
| WO2017134594A1 (en) * | 2016-02-04 | 2017-08-10 | Apharm S.R.L. | New topical compositions comprising usnic acid and their use in therapy |
| CN106943341A (en) * | 2017-05-10 | 2017-07-14 | 重庆理工大学 | A kind of external preparation for improving usnic acid Transdermal absorption and its application in skin wound healing is promoted |
Non-Patent Citations (1)
| Title |
|---|
| Usnic acid and its derivatives for pharmaceutical use: a patent review (2000-2017);Olga A. Luzina 等;《Expert Opinion on Therapeutic Patents》;20180509;全文 * |
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