CN114432235B - Preparation method of difunctional slow-release supermolecule hydrogel for injection - Google Patents
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Abstract
The invention provides a preparation method of a difunctional slow-release type supermolecule hydrogel for injection, which comprises the following steps: step 1: extracting radix Scutellariae with ethanol under ultrasonic condition to obtain radix Scutellariae extract; step 2: dissolving chiral gel factor LBA with ethanol to prepare high-concentration stock solution; step 3: mixing Scutellariae radix extract with chiral gel factors of different concentrations; step 3: adding deionized water into the mixed solution, and standing to form the gel. The chiral supramolecular hydrogel is used as a gelling agent, the baical skullcap root extract is used as a functional substance, the former is generated through non-covalent bond interaction with small molecules in the baical skullcap root extract, other organic solvents, stabilizers and other substances are not needed to be added in the preparation process, and the preparation process is simple, mild, green, safe and nontoxic, and ensures the safety of operators.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a preparation method of a difunctional slow-release type supermolecule hydrogel for injection.
Background
Inflammatory bowel disease (inflammatory bowel disease, IBD) is a chronic non-specific disease with an undefined pathogenesis and mainly involves the intestinal tract, and in recent years, the number of people suffering from IBD in China is on an increasing trend, and the demand for therapeutic drugs is also increasing. Although a great deal of research results have been applied to the treatment of IBD, to some extent, the effects of long-term maintenance and alleviation, promotion of tissue healing, reduction of hospitalization rate and operation rate are achieved, there are many adverse reactions and potential safety hazards, such as inhibition of human immune function, bacterial resistance, etc. The Chinese medicine has the functions of regulating intestinal flora disorder, maintaining intestinal flora steady state and diversity, and has positive effects on IBD treatment, such as spleen invigorating and intestine benefiting pill, red intestine relieving and exogenously clearing pill, compound kuh-seng enteritis rehabilitation tablet, etc. However, the material basis of the action of traditional Chinese medicine is not clear, which hinders the further development of traditional Chinese medicine treatment. Systematic research on single traditional Chinese medicines becomes a trend of disease treatment, and the common property of the three traditional Chinese medicine compounds is inspired, and the discovery that the traditional Chinese medicine compounds all contain the baikal skullcap root indicates that the baikal skullcap root has a certain potential application value for treating enteritis. In fact, the radix Scutellariae slice is currently applied to the treatment of related diseases such as inflammation diminishing and detoxification, however, the absorption performance of the radix Scutellariae slice is poor, which affects the use of the radix Scutellariae slice as a medicament for treating IBD.
The baical skullcap root contains a plurality of molecules with potential therapeutic effects, such as baicalein, wogonin, baicalin, oroxylin and the like, and has been reported to be applied to the fields of antibiosis and anti-inflammatory. The traditional Chinese medicine has multi-target effect, and the molecules can act synergistically. The use of a single molecule for disease treatment is difficult to address interactions between multiple targets, and thus co-delivery of multiple small active molecules is an attractive area of research for the treatment of IBD. The supermolecular hydrogel has wide medical application prospect, the supermolecular hydrogel system has a plurality of binding sites, can be combined with guest molecules through non-covalent bond interaction, and can generate reversible responsiveness to external environment due to weaker combining capability. Unfortunately, there is no current research on the multicomponent co-delivery of drugs by supramolecular hydrogels.
Disclosure of Invention
The invention aims at solving the problems existing in the prior art, provides a preparation method of a difunctional slow-release type supermolecule hydrogel for injection, and particularly relates to a preparation method of a supermolecule hydrogel co-delivery system based on chiral characteristics. The method has simple preparation process, safety, environmental protection, and antibacterial, antioxidant and long-acting release functions.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a difunctional slow-release type supermolecule hydrogel for injection, which comprises the following steps:
s1, weighing radix scutellariae, grinding and extracting to obtain radix scutellariae extract;
s2, weighing supermolecule chiral gel factors, and adding ethanol to prepare high-concentration stock solution;
s3, uniformly mixing the high-concentration stock solution with the scutellaria baicalensis extracting solution, and then adding deionized water;
s4, standing to obtain the supermolecule hydrogel.
As an embodiment of the present invention, the method of extraction in step S1 specifically includes: adding ethanol into crushed radix Scutellariae, ultrasonic extracting at 40-70deg.C for 40-60 min at a ratio of 10:40-50, repeating the extraction for 4-5 times, mixing the extractive solutions, and concentrating to obtain radix Scutellariae extractive solution.
As an embodiment of the present invention, the root of scutellaria baicalensis in step S1 is a dried, processed root of scutellaria baicalensis.
As an embodiment of the present invention, the supramolecular chiral gelator in step S2 is LBA, and the structure is as follows:
as one embodiment of the present invention, the concentration of chiral gelator LBA in the high concentration stock solution in step S2 is 25-35mg/ml. The concentration is preferably 30mg/ml.
As one embodiment of the present invention, the volume ratio of the high concentration stock solution to the scutellaria baicalensis extract in the step S3 is 1:1.5-1:3.5. The volume ratio of the high concentration stock solution to the scutellaria baicalensis extract is preferably 1:2.8. When the volume ratio is too large, the mechanical strength of the gel is lowered, possibly resulting in burst release of the supported substance.
As one embodiment of the invention, the volume of deionized water in the step S3 is 5-10 times of the volume of the mixed high-concentration stock solution and the scutellaria baicalensis extracting solution. The volume ratio is preferably 7 times.
As an embodiment of the present invention, the supramolecular hydrogel in step S4 is a pale yellow gel.
The invention also provides a preparation method of the difunctional slow-release type supermolecule solution for injection, which comprises the following steps:
a1, weighing radix scutellariae, grinding and extracting to obtain radix scutellariae extract;
a2, weighing chiral gel factor LBA, and adding ethanol to prepare high-concentration stock solution;
a3, uniformly mixing the high-concentration stock solution with the scutellaria baicalensis extracting solution to obtain the solution.
The hydrogel injected by the solution can be gelled instantaneously, and is convenient for slow administration.
The invention provides a difunctional slow-release type supermolecule hydrogel which is prepared by the preparation method and can be used for injection.
The invention provides a difunctional slow-release type supermolecule solution which is prepared by the preparation method and can be used for injection.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the preparation method of the supramolecular hydrogel based on chiral characteristics, provided by the invention, the dressing is endowed with the antioxidant, anti-inflammatory and antibacterial properties by adopting the baical skullcap root extract, and the chiral gel factor LBA is taken as a gelling agent, so that a plurality of active molecules can be loaded simultaneously to exert the treatment effect, other reactions are not required to be introduced in the preparation process, and the preparation process is simple and mild, green, safe and nontoxic, and ensures the safety of operators; the hydrogel prepared by the invention has good antioxidation and antibacterial properties and long-acting slow release performance;
2. the hydrogel prepared by the invention has simple components and easy preparation;
3. although the prior patent (CN 112641995B) also uses the supermolecular gel and the traditional Chinese medicine components of the patent, the obtained hydrogel is a gel block with high strength, is suitable for wound repair and is not suitable for enteritis treatment. The supermolecular gel system prepared by the invention has the characteristic of rapid gelation, and can be applied to enteritis.
Drawings
Other features, objects and advantages of the present invention will become more apparent upon reading of the detailed description of non-limiting embodiments, given with reference to the accompanying drawings in which:
FIG. 1 is a schematic diagram of an example preparation gel and an antibacterial test thereof, wherein A is a preparation appearance diagram of a bifunctional supramolecular hydrogel; b is a preparation appearance diagram of the difunctional supermolecule hydrogel; c is an antibacterial diagram test schematic diagram of the supramolecular hydrogel;
FIG. 2 is a graph of radical scavenging for supramolecular hydrogels prepared at different volume ratios;
figure 3 is a graph showing the effect of different volume ratios of hydrogels on slow release of active molecules.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The following examples, which are presented to provide those of ordinary skill in the art with a detailed description of the invention and to provide a further understanding of the invention, are presented in terms of implementation and operation. It should be noted that the protection scope of the present invention is not limited to the following embodiments, and several adjustments and improvements made on the premise of the inventive concept are all within the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of a bifunctional supermolecule hydrogel, which comprises the following steps:
step 1: weighing 10g of radix scutellariae, grinding, adding 40mL of ethanol, carrying out ultrasonic treatment, filtering, collecting filtrate, repeatedly extracting for 4 times, and concentrating under reduced pressure to 50mL to obtain radix scutellariae extract;
step 2: weighing LBA, adding ethanol, and preparing 30mg/ml stock solution;
step 3: uniformly mixing 100 mu L of LBA high-concentration stock solution and baical skullcap root extract (200 mu L), and then adding deionized water with the volume of 7 times;
step 4: after standing, a supramolecular hydrogel can be obtained, as shown in FIG. 1A. The obtained gel is stable and can load the added Chinese medicinal extract. The antibacterial activity is shown in figure 1C, the free radical scavenging activity is shown in figure 2, and the long-acting release function is shown in figure 3.
Example 2
The preparation method of the bifunctional supermolecule hydrogel comprises the following steps:
step 1: weighing 10g of radix scutellariae, grinding, adding 40mL of ethanol, carrying out ultrasonic treatment, filtering, collecting filtrate, repeatedly extracting for 4 times, and concentrating under reduced pressure to 50mL to obtain radix scutellariae extract;
step 2: weighing LBA, adding ethanol, and preparing 30mg/ml stock solution;
step 3: uniformly mixing 100 mu L of LBA high-concentration stock solution with the baical skullcap root extract (230 mu L), and then adding deionized water with the volume of 7 times;
step 4: after standing, the supermolecule hydrogel can be obtained as shown in figure 1A, and has the activity of scavenging free radicals (figure 2) and long-acting release function (figure 3).
Example 3
The preparation method of the bifunctional supermolecule hydrogel comprises the following steps:
step 1: weighing 10g of radix scutellariae, grinding, adding 40mL of ethanol, carrying out ultrasonic treatment, filtering, collecting filtrate, repeatedly extracting for 4 times, and concentrating under reduced pressure to 50mL to obtain radix scutellariae extract;
step 2: weighing LBA, adding ethanol, and preparing 30mg/ml stock solution;
step 3: uniformly mixing 100 mu L of LBA high-concentration stock solution and baical skullcap root extract (250 mu L), and then adding deionized water with the volume of 7 times;
step 4: after standing, the supermolecular hydrogel can be obtained as shown in figure 1A, and has antibacterial (figure 1C), free radical scavenging activity (figure 2) and long-acting release function (figure 3).
Example 4
The preparation method of the bifunctional supermolecule hydrogel comprises the following steps:
step 1: weighing 10g of radix scutellariae, grinding, adding 40mL of ethanol, carrying out ultrasonic treatment, filtering, collecting filtrate, repeatedly extracting for 4 times, and concentrating under reduced pressure to 50mL to obtain radix scutellariae extract;
step 2: weighing LBA, adding ethanol, and preparing 30mg/ml stock solution;
step 3: uniformly mixing 100 mu L of LBA high-concentration stock solution and baical skullcap root extract (280 mu L), and then adding deionized water with the volume of 7 times;
step 4: after standing, the supermolecular hydrogel can be obtained as shown in figure 1B, and has the functions of resisting bacteria (figure 1C), scavenging free radical activity (figure 2) and long-acting release (figure 3).
Example 5
The preparation method of the bifunctional supermolecule hydrogel comprises the following steps:
step 1: weighing 10g of radix scutellariae, grinding, adding 40mL of ethanol, carrying out ultrasonic treatment, filtering, collecting filtrate, repeatedly extracting for 4 times, and concentrating under reduced pressure to 50mL to obtain radix scutellariae extract;
step 2: weighing LBA, adding ethanol, and preparing 30mg/ml stock solution;
step 3: uniformly mixing 100 mu L of LBA high-concentration stock solution and baical skullcap root extract (300 mu L), and then adding deionized water with the volume of 7 times;
step 4: and standing to obtain the supermolecule hydrogel.
Example 6
The preparation method of the bifunctional supermolecule hydrogel comprises the following steps:
step 1: weighing 10g of radix scutellariae, grinding, adding 40mL of ethanol, carrying out ultrasonic treatment, filtering, collecting filtrate, repeatedly extracting for 4 times, and concentrating under reduced pressure to 50mL to obtain radix scutellariae extract;
step 2: weighing LBA, adding ethanol, and preparing 30mg/ml stock solution;
step 3: uniformly mixing 100 mu L of LBA high-concentration stock solution and baical skullcap root extract (320 mu L), and then adding deionized water with the volume of 7 times;
step 4: and standing to obtain the supermolecule hydrogel.
Hydrogels prepared in examples 3 and 4 at different volume ratios are shown in FIG. 1B, and the resulting gels have yellow samples exuded at volume ratios of 1:3.0 and 1:3.2, indicating that all of the added herbal extract cannot be loaded at this ratio.
Example 7
The preparation method of the bifunctional supramolecular hydrogel is basically the same as that of example 1, except that: the supramolecular hydrogel factor is DB3. Molecular formula is shown as
The strength of the co-assembled gel obtained by the supramolecular hydrogel factor DB3 is weaker, and the release rate of drug molecules is obviously accelerated. The medicine cannot be effectively adhered to the wall of the bottle after being injected into water, has inferior effect of adhering to the stomach wall as compared with LBA, and is not beneficial to the stable release of the medicine molecules in the later period.
The foregoing describes specific embodiments of the present invention. It is to be understood that the invention is not limited to the particular embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the claims without affecting the spirit of the invention.
Claims (8)
1. The preparation method of the difunctional slow-release type supermolecule hydrogel for injection is characterized by comprising the following steps of:
s1, weighing radix scutellariae, grinding and extracting to obtain radix scutellariae extract;
s2, weighing supermolecule chiral gel factors, and adding ethanol to prepare high-concentration stock solution;
s3, uniformly mixing the high-concentration stock solution with the scutellaria baicalensis extracting solution, and then adding deionized water;
s4, standing to obtain supermolecule hydrogel;
the extraction method in the step S1 specifically comprises the following steps: adding ethanol into crushed radix Scutellariae, ultrasonic extracting at 40-70deg.C for 40-60 min at a feed liquid ratio of 10g to 40-50 mL for 4-5 times, mixing the extractive solutions, and concentrating to obtain radix Scutellariae extractive solution;
in the step S2, the supramolecular chiral gel factor is LBA, and the structure is as follows:
2. the preparation method according to claim 1, wherein the baical skullcap root in step S1 is dried processed baical skullcap root.
3. The method according to claim 1, wherein the concentration of chiral gelator LBA in the high concentration stock solution in step S2 is 25-35mg/ml.
4. The preparation method according to claim 1, wherein the volume ratio of the high concentration stock solution to the scutellaria baicalensis extracting solution in the step S3 is 1:1.5-1:3.5.
5. The preparation method according to claim 1, wherein the volume of deionized water in step S3 is 5-10 times the volume of the high concentration stock solution mixed with the scutellaria baicalensis extract.
6. A method for preparing a bifunctional slow-release supermolecule solution for injection, which is characterized by comprising the following steps:
a1, weighing radix scutellariae, grinding and extracting to obtain radix scutellariae extract;
a2, weighing chiral gel factor LBA, and adding ethanol to prepare high-concentration stock solution;
a3, uniformly mixing the high-concentration stock solution with the scutellaria baicalensis extracting solution to obtain a solution;
the extraction method in the step A1 specifically comprises the following steps: adding ethanol into crushed radix Scutellariae, ultrasonic extracting at 40-70deg.C for 40-60 min at a feed liquid ratio of 10g to 40-50 mL for 4-5 times, mixing the extractive solutions, and concentrating to obtain radix Scutellariae extractive solution;
the structure of the LBA in step A2 is as follows:
7. a bifunctional sustained-release supramolecular hydrogel for injection prepared by the preparation method of claim 1.
8. A bifunctional sustained-release supramolecular solution for injection prepared by the preparation method of claim 6.
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