CN111643567A - Pricklyash peel volatile oil inclusion compound oral tablet and preparation method thereof - Google Patents

Pricklyash peel volatile oil inclusion compound oral tablet and preparation method thereof Download PDF

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CN111643567A
CN111643567A CN202010645054.9A CN202010645054A CN111643567A CN 111643567 A CN111643567 A CN 111643567A CN 202010645054 A CN202010645054 A CN 202010645054A CN 111643567 A CN111643567 A CN 111643567A
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volatile oil
pepper
parts
inclusion compound
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刘娜
赵毅
车彦云
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Yunnan University of Traditional Chinese Medicine TCM
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Abstract

The application discloses a pricklyash peel volatile oil inclusion compound oral tablet and a preparation method thereof, wherein the pricklyash peel volatile oil inclusion compound oral tablet comprises, by mass, 4-6 parts of pricklyash peel volatile oil, 50-60 parts of beta-cyclodextrin, 40-50 parts of a diluent, 0.25-1 part of polyvinylpyrrolidone and 4-6 parts of talcum powder. One technical effect of the present application is that the present application can enhance the stability of the volatile oil, reduce volatilization, mask unpleasant odors, and facilitate patient administration and carrying.

Description

Pricklyash peel volatile oil inclusion compound oral tablet and preparation method thereof
Technical Field
The application belongs to the technical field of health-care products, and particularly relates to a pepper volatile oil inclusion compound oral tablet and a preparation method thereof.
Background
The pericarpium Zanthoxyli is dried mature pericarp of Zanthoxylum Bungeanum (Zanthoxylum Bungeanum Maxim) and green pepper (Z.Schinifolium Sieb.et Zucc.) belonging to genus Zanthoxylum of family Rutaceae. It is recorded in the first part of the 2015 edition of Chinese pharmacopoeia and has the efficacies of warming middle-jiao to relieve pain, killing parasites to relieve itching. Is clinically used for treating retention of food and drink, cold pain of heart and abdomen, cough, reversed flow of qi, cold and damp evil, vomiting, diarrhea, dysentery, toothache, ascariasis pain, pruritus vulvae and other symptoms. The pricklyash peel volatile oil has strong pharmacological activity in the aspects of anti-inflammation, bacteriostasis, disinsection, tumor resistance and the like. The volatile oil of fructus Zanthoxyli also contains a large amount of medicinal effective components, and has cardiovascular pharmacological activities of resisting oxidation, regulating blood lipid, resisting platelet, resisting thrombi, regulating immunity, lowering blood pressure, and protecting stress myocardial injury. For example, the relatively less polar component of the volatile oil of Zanthoxylum piperitum has effect in inhibiting fungi, and the relatively more polar component has effect in inhibiting bacteria.
The Chinese prickly ash is orally taken in the traditional use, the Chinese prickly ash is contained in the mouth and has irritation, and the content of the Chinese prickly ash volatile oil is not high. Because the content is not high, the pepper volatile oil is not suitable to be prepared into simple soft capsules, and the dosage of one-time administration is too large. The volatile oil has the defects of easy volatilization, easy oxidation, difficult stable existence, poor water solubility, peculiar smell and the like, and the application of the volatile oil in the aspect of medicine is greatly limited. Therefore, the need exists for an oral tablet containing the volatile oil inclusion compound of the pepper.
Disclosure of Invention
One purpose of the application is to provide a technical scheme of the internal tablet containing the volatile oil inclusion compound of the pepper.
According to one aspect of the application, the application provides an internal tablet of a volatile oil inclusion compound of pepper, which comprises, by mass, 4-6 parts of volatile oil of pepper, 50-60 parts of beta-cyclodextrin, 40-50 parts of a diluent, 0.25-1 part of polyvinylpyrrolidone and 4-6 parts of talcum powder.
Optionally, the Chinese prickly ash oil comprises, by mass, 5 parts of Chinese prickly ash volatile oil, 56 parts of beta-cyclodextrin, 44 parts of a diluent, 0.5 part of polyvinylpyrrolidone and 5 parts of talcum powder.
Optionally, the diluent is dextrin and microcrystalline cellulose, and the mass ratio of the dextrin to the microcrystalline cellulose is 2: 1.
According to another aspect of the application, the application also provides a preparation method of the pericarpium zanthoxyli volatile oil inclusion compound oral tablet, which comprises the following steps:
providing pepper volatile oil, beta-cyclodextrin, dextrin + MCC, polyvinylpyrrolidone and talcum powder;
preparing a pepper volatile oil inclusion compound by using pepper volatile oil and beta-cyclodextrin;
preparing a polyvinylpyrrolidone ethanol solution with the concentration of 5% by using polyvinylpyrrolidone;
mixing the fructus Zanthoxyli volatile oil clathrate with diluent and polyvinylpyrrolidone ethanol solution, granulating, drying, sieving, adding pulvis Talci, mixing, and tabletting to obtain fructus Zanthoxyli volatile oil clathrate oral tablet.
Optionally, the pepper volatile oil is prepared by the following method:
weighing pericarpium Zanthoxyli coarse powder, adding 8 times of water, soaking for 1 hr, extracting by steam distillation, refrigerating, and oil-water separating to obtain pericarpium Zanthoxyli volatile oil.
Optionally, the inclusion compound of the pepper volatile oil is prepared by the following method:
adding water into the beta-cyclodextrin to prepare a beta-cyclodextrin saturated aqueous solution;
dissolving the pepper volatile oil in absolute ethyl alcohol, and mixing with a beta-cyclodextrin saturated aqueous solution to obtain a mixed solution;
and (3) placing the mixed solution in an ultrasonic instrument for ultrasonic treatment, refrigerating the mixed solution after ultrasonic treatment, then performing suction filtration, and drying a filter cake to obtain the pepper volatile oil inclusion compound.
Optionally, the parameters of the ultrasonic treatment are power 350W and ultrasonic time 45 min.
Optionally, the mixed liquor is refrigerated for 12 h.
Optionally, the filter cake is dried at room temperature for 24 h.
Optionally, the specific method of sieving after drying is drying in a drying oven at 45 ℃, and sieving by a second sieve to complete granules after drying is completed.
Optionally, the wetting agent is a 75% ethanol solution.
One technical effect of the present application is that the present application can enhance the stability of the volatile oil, reduce volatilization, mask unpleasant odors, and facilitate patient administration and carrying.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1 shows the essential oil of Zanthoxylum bungeanum prepared in example 1 of the present application;
FIG. 2 shows a clathrate of essential oil of Zanthoxylum bungeanum prepared in example 1 of the present application;
FIG. 3 shows an oral tablet of essential oil of Zanthoxylum bungeanum prepared in example 1 of the present application.
Detailed Description
Embodiments of the present application will be described in detail with reference to the drawings and examples, so that how to implement technical means to solve technical problems and achieve technical effects of the present application can be fully understood and implemented.
Example 1
Weighing pericarpium Zanthoxyli coarse powder, adding 8 times of water, soaking for 1 hr, extracting by steam distillation, refrigerating, and oil-water separating to obtain pericarpium Zanthoxyli volatile oil.
Weighing 5 parts of pepper volatile oil, 56 parts of beta-cyclodextrin, 44 parts of diluent, 0.5 part of polyvinylpyrrolidone and 5 parts of talcum powder. The diluent is dextrin and microcrystalline cellulose, and the mass ratio of the dextrin to the microcrystalline cellulose is 2: 1.
Adding water into the beta-cyclodextrin to prepare a beta-cyclodextrin saturated aqueous solution;
dissolving the pepper volatile oil in absolute ethyl alcohol, and mixing with a beta-cyclodextrin saturated aqueous solution to obtain a mixed solution;
putting the mixed solution into an ultrasonic instrument for ultrasonic treatment, wherein the ultrasonic power is 350W, and the ultrasonic time is 45 min; refrigerating the mixed solution after ultrasonic treatment for 12h, then carrying out suction filtration, and drying the filter cake for 24h at room temperature to obtain the pepper volatile oil inclusion compound.
Preparing a polyvinylpyrrolidone ethanol solution with the concentration of 5% by using polyvinylpyrrolidone;
mixing the fructus Zanthoxyli volatile oil clathrate with diluent and polyvinylpyrrolidone ethanol solution, adding wetting agent (75% ethanol solution) for granulating, drying at 45 deg.C in drying oven, sieving with second sieve, adding pulvis Talci, mixing, and tabletting with rotary tablet press to obtain fructus Zanthoxyli volatile oil clathrate oral tablet.
Steam distillation is an extraction method in which a plant material containing volatile components is co-distilled with water to distill off the volatile components along with the steam, and the volatile components are separated by condensation. Steam distillation is suitable for separating and purifying some substances which have high boiling points and are easy to decompose and destroy, and is used for separating volatile liquid or solid substances which are not soluble with water. An organic compound and its purification, which is suitable for extracting the active components of plant which is volatile, can be distilled without being destroyed by steam, and is stable in water and insoluble in water or water.
According to the application, the pepper volatile oil is embedded into the cyclodextrin cylindrical structure to form an ultrafine particle dispersion, so that the original properties and effects of the medicament can be guaranteed, and the converted carbohydrate can be effectively absorbed by a human body and directly participates in the metabolic process of the human body. The inclusion compound is rarely influenced by the outside, exists in a balanced state, has good stability, and simultaneously increases the stability of the medicine to a certain extent. The volatile oil of the pepper is encapsulated in the beta-cyclodextrin, so that the unpleasant odor of the volatile oil of the pepper can be covered, the irritation caused by directly taking the volatile oil of the pepper is reduced, and the stability of the volatile oil of the pepper in the buccal tablet is improved. The volatile oil of the pepper is prepared into the inclusion compound of the volatile oil of the pepper, so that the solubility and the dissolution rate of the volatile oil can be increased, the unpleasant smell of the volatile oil of the pepper can be covered, the irritation of the volatile oil of the pepper can be reduced, the volatile oil of the pepper is volatile, the stability of the inclusion compound prepared can be improved, and conditions are provided for preparing the buccal tablet. The pepper volatile oil is prepared into a solid preparation, so that the effective components in the pepper volatile oil are enriched while the pepper volatile oil is convenient to transport, store and take.
Bacteriostatic activity experiment of pepper volatile oil prepared based on example 1
1.1 culture Medium and Strain
Reagent testing: the positive control drug fluconazole for antifungal activity detection is dissolved in DMSO, centrifuged to obtain supernatant, stored at the concentration of 50mg/mL, sealed at 4 ℃ and stored in a dark place.
1.1.1 culture Medium
(1) Saxifrage liquid medium: 10.0g of peptone and 40.0g of glucose were dissolved in 1000ml of distilled water, and autoclaved at 115 ℃ for 30 minutes for use.
(2) Sabouraud solid medium: 10.0g of peptone, 40.0g of glucose and 20g of agar were dissolved in 1000ml of distilled water, and autoclaved at 115 ℃ for 30 minutes for use.
(3) Methylene blue M-H agar medium: M-H agar + 2% glucose +0.5ug/ml methylene blue, and autoclaving at 121 deg.C for 15 min.
(4) LB liquid medium: accurately weighing 10g of tryptone, 5g of yeast extract and 10g of sodium chloride, placing the tryptone, the yeast extract and the sodium chloride into a 1000mL blue-covered reagent bottle, fixing the volume to 1000mL by using distilled water, and carrying out autoclaving at 121 ℃ for 15min for later use.
(5) LB solid medium: accurately weighing 10g of tryptone, 5g of yeast extract, 10g of sodium chloride and 15g of agar, placing the weighed materials into a 1000mL blue-covered reagent bottle, fixing the volume to 1000mL by using distilled water, and carrying out autoclaving at 121 ℃ for 15min for later use.
1.1.2 strains
Candida albicans standard strain SC5314, Candida albicans clinical isolation drug-resistant strain 23#, Staphylococcus aureus and Escherichia coli.
1.2 antibacterial test method K-B method (Standard filter paper sheet method)
1.2.1 taking a pure bacterial colony cultured for 16-18 h at 37 ℃ on a culture medium, preparing bacterial suspension, adjusting the concentration to be 1 multiplied by 107CFU/mL, loading 500uL of bacterial liquid on each flat plate, immediately and uniformly coating the plate with a cotton swab, placing for about 10 minutes, and loading a sterile filter paper sheet with the diameter of 6mm by using a pair of tweezers when the bacterial liquid is completely absorbed by the flat plate.
1.2.2 after loading the paper sheet, loading a certain amount of sample to be tested on the center of the paper filter sheet to prevent the bacteria inhibition zone from deforming, after the sample is uniformly and completely absorbed, putting the sample into a constant temperature and humidity box or a CO2 incubator, generally, after incubating for 18-24h (fungi) or 12-16h (bacteria), checking each flat plate, if the inoculation flat plate is satisfied, the bacteria inhibition zone should be in a perfect circle shape, and bacterial colonies should be fused with each other to grow. The diameter edge of the antibacterial ring is measured to be 80% inhibited, and if the colony grows weakly, the culture is continued for 20-24 h.
1.2.3 reading the diameter of the inhibition zone under the black background without reflecting light, wherein the diameter of the inhibition zone comprises the diameter of the paper sheet. The limit of the inhibition zone should be an area where no obvious visible fungus growth is observed by naked eyes, and tiny colonies which grow weakly at the edge of the inhibition zone and can only be observed under a magnifying glass should be ignored.
1.3 results of bacteriostatic tests
The pepper volatile oil prepared in example 1 has activity on candida albicans standard strain SC5314, candida albicans clinical drug-resistant strain 23#, staphylococcus aureus and escherichia coli.
Example 2
Weighing pericarpium Zanthoxyli coarse powder, adding 8 times of water, soaking for 1 hr, extracting by steam distillation, refrigerating, and oil-water separating to obtain pericarpium Zanthoxyli volatile oil.
Weighing 4 parts of pepper volatile oil, 50 parts of beta-cyclodextrin, 40 parts of diluent, 0.25 part of polyvinylpyrrolidone and 4 parts of talcum powder. The diluent is dextrin and microcrystalline cellulose, and the mass ratio of the dextrin to the microcrystalline cellulose is 2: 1.
Adding water into the beta-cyclodextrin to prepare a beta-cyclodextrin saturated aqueous solution;
dissolving the pepper volatile oil in absolute ethyl alcohol, and mixing with a beta-cyclodextrin saturated aqueous solution to obtain a mixed solution;
putting the mixed solution into an ultrasonic instrument for ultrasonic treatment, wherein the ultrasonic power is 350W, and the ultrasonic time is 45 min; refrigerating the mixed solution after ultrasonic treatment for 12h, then carrying out suction filtration, and drying the filter cake for 24h at room temperature to obtain the pepper volatile oil inclusion compound.
Preparing a polyvinylpyrrolidone ethanol solution with the concentration of 5% by using polyvinylpyrrolidone;
mixing the fructus Zanthoxyli volatile oil clathrate with diluent and polyvinylpyrrolidone ethanol solution, adding wetting agent (75% ethanol solution) for granulating, drying at 45 deg.C in drying oven, sieving with second sieve, adding pulvis Talci, mixing, and tabletting with rotary tablet press to obtain fructus Zanthoxyli volatile oil clathrate oral tablet.
Example 3
Weighing pericarpium Zanthoxyli coarse powder, adding 8 times of water, soaking for 1 hr, extracting by steam distillation, refrigerating, and oil-water separating to obtain pericarpium Zanthoxyli volatile oil.
Weighing 6 parts of pepper volatile oil, 60 parts of beta-cyclodextrin, 50 parts of diluent, 1 part of polyvinylpyrrolidone and 6 parts of talcum powder. The diluent is dextrin and microcrystalline cellulose, and the mass ratio of the dextrin to the microcrystalline cellulose is 2: 1.
Adding water into the beta-cyclodextrin to prepare a beta-cyclodextrin saturated aqueous solution;
dissolving the pepper volatile oil in absolute ethyl alcohol, and mixing with a beta-cyclodextrin saturated aqueous solution to obtain a mixed solution;
putting the mixed solution into an ultrasonic instrument for ultrasonic treatment, wherein the ultrasonic power is 350W, and the ultrasonic time is 45 min; refrigerating the mixed solution after ultrasonic treatment for 12h, then carrying out suction filtration, and drying the filter cake for 24h at room temperature to obtain the pepper volatile oil inclusion compound.
Preparing a polyvinylpyrrolidone ethanol solution with the concentration of 5% by using polyvinylpyrrolidone;
mixing the fructus Zanthoxyli volatile oil clathrate with diluent and polyvinylpyrrolidone ethanol solution, adding wetting agent (75% ethanol solution) for granulating, drying at 45 deg.C in drying oven, sieving with second sieve, adding pulvis Talci, mixing, and tabletting with rotary tablet press to obtain fructus Zanthoxyli volatile oil clathrate oral tablet.
As used in the specification and claims, certain terms are used to refer to particular components or methods. As one skilled in the art will appreciate, different regions may refer to a component by different names. The present specification and claims do not intend to distinguish between components that differ in name but not in name. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, and a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect. The description which follows is a preferred embodiment of the present application, but is made for the purpose of illustrating the general principles of the application and not for the purpose of limiting the scope of the application. The protection scope of the present application shall be subject to the definitions of the appended claims.
It is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a good or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such good or system. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a commodity or system that includes the element.
While the foregoing description shows and describes several preferred embodiments of the invention, it is to be understood, as noted above, that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of 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 (10)

1. An oral tablet of volatile oil inclusion compound of pepper is characterized by comprising, by mass, 4-6 parts of volatile oil of pepper, 50-60 parts of beta-cyclodextrin, 40-50 parts of diluent, 0.25-1 part of polyvinylpyrrolidone and 4-6 parts of talcum powder.
2. The Chinese prickly ash volatile oil inclusion compound oral tablet according to claim 1, which is characterized by comprising, by mass, 5 parts of Chinese prickly ash volatile oil, 56 parts of beta-cyclodextrin, 44 parts of a diluent, 0.5 part of polyvinylpyrrolidone and 5 parts of talcum powder.
3. The internal tablet of the inclusion compound of pepper volatile oil as claimed in claim 1, wherein the diluent is dextrin and microcrystalline cellulose, and the mass ratio of the dextrin to the microcrystalline cellulose is 2: 1.
4. A preparation method of the prickly ash volatile oil inclusion compound oral tablet as claimed in any one of claims 1 to 3, which is characterized by comprising the following steps:
providing pepper volatile oil, beta-cyclodextrin, a diluent, polyvinylpyrrolidone and talcum powder;
preparing a pepper volatile oil inclusion compound by using pepper volatile oil and beta-cyclodextrin;
preparing a polyvinylpyrrolidone ethanol solution with the concentration of 5% by using polyvinylpyrrolidone;
mixing the fructus Zanthoxyli volatile oil clathrate with diluent and polyvinylpyrrolidone ethanol solution, granulating, drying, sieving, adding pulvis Talci, mixing, and tabletting to obtain fructus Zanthoxyli volatile oil clathrate oral tablet.
5. The preparation method according to claim 4, wherein the pericarpium zanthoxyli volatile oil is prepared by the following method:
weighing pericarpium Zanthoxyli coarse powder, adding 8 times of water, soaking for 1 hr, extracting by steam distillation, refrigerating, and oil-water separating to obtain pericarpium Zanthoxyli volatile oil.
6. The preparation method according to claim 4, wherein the inclusion compound of the pepper volatile oil is prepared by the following steps:
adding water into the beta-cyclodextrin to prepare a beta-cyclodextrin saturated aqueous solution;
dissolving the pepper volatile oil in absolute ethyl alcohol, and mixing with a beta-cyclodextrin saturated aqueous solution to obtain a mixed solution;
and (3) placing the mixed solution in an ultrasonic instrument for ultrasonic treatment, refrigerating the mixed solution after ultrasonic treatment, then performing suction filtration, and drying a filter cake to obtain the pepper volatile oil inclusion compound.
7. The preparation method according to claim 6, wherein the ultrasonic treatment parameters are power 350W and ultrasonic time 45 min.
8. The method according to claim 6, wherein the mixed solution is refrigerated for 12 hours, and the filter cake is dried at room temperature for 24 hours.
9. The process according to claim 3, wherein the specific method of sieving after drying is drying in a 45 ℃ drying oven, and sieving with a second sieve to complete the granules after completion of the drying.
10. The method of claim 3, wherein the wetting agent is a 75% ethanol solution.
CN202010645054.9A 2020-07-07 2020-07-07 Pricklyash peel volatile oil inclusion compound oral tablet and preparation method thereof Withdrawn CN111643567A (en)

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Cited By (1)

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CN114404612A (en) * 2020-10-28 2022-04-29 西南交通大学 Zanthoxylum bungeanum oleosin cyclodextrin inclusion compound and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114404612A (en) * 2020-10-28 2022-04-29 西南交通大学 Zanthoxylum bungeanum oleosin cyclodextrin inclusion compound and preparation method thereof
CN114404612B (en) * 2020-10-28 2024-03-29 西南交通大学 Zanthoxylum oil cyclodextrin inclusion compound and preparation method thereof

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