CN111704680B - Tellurium-doped chitosan material - Google Patents
Tellurium-doped chitosan material Download PDFInfo
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- CN111704680B CN111704680B CN202010566185.8A CN202010566185A CN111704680B CN 111704680 B CN111704680 B CN 111704680B CN 202010566185 A CN202010566185 A CN 202010566185A CN 111704680 B CN111704680 B CN 111704680B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
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Abstract
The invention relates to a tellurium-doped chitosan material, which comprises the following synthetic steps: firstly, tellurium powder and n-butyl lithium solution are reacted to synthesize butyl tellurium lithium solution, and then the solution is mixed with chitosan according to the mass ratio of tellurium to chitosan being 0.01% -0.2%: 1, and soaking the chitosan to load tellurium element. In the material, the mass content of tellurium is between 0.0011 and 0.016 percent. The material has the characteristic of sterilization under the drive of mild low-energy light (such as red light), and can be used for manufacturing antibacterial materials.
Description
Technical Field
The invention relates to a tellurium-doped chitosan material, belonging to the technical field of antibacterial materials.
Background
The novel antibacterial material is a cross discipline frontier field combining material chemistry and medicine, and has wide market application prospect. For example, nano silver antibacterial materials are widely used due to their high-efficiency and broad antibacterial properties, and many products are already on the market. However, recently, nano silver is found to have certain cytotoxicity, so that related products are put on the shelf successively, and therefore, the vacant market space is filled up, and the development of a novel antibacterial material has a good application value.
On the other hand, tellurium is a relatively rare dispersive element and is mainly applied to the metallurgical industry. Tellurium is a chalcogen with properties similar to sulfur and selenium. With the research on chalcogen elements, some properties of tellurium elements are gradually mastered. For example, the subject group has recently found that tellurium element is easy to generate homolytic cleavage to generate free radical due to more fragile chemical bond, and can catalyze the oxidation deoximation reaction under mild conditions (Science Bulletin,2019,64, 1280-. The fragile property of tellurium-containing chemical bonds makes it a more excellent oxygen-carrying catalyst for catalyzing molecular oxygen to oxidize organic substances (similar to selenium-catalyzed reactions which require the use of hydrogen peroxide oxidants).
Disclosure of Invention
The invention aims to provide a tellurium-doped chitosan material. The material is prepared by taking cheap and easily-obtained chitosan as a main material and performing lithium telluride on n-butyl tellurium. The material can be sterilized under the drive of low-energy light (such as red light), and is expected to be used for manufacturing some antibacterial materials.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a tellurium-doped chitosan material is prepared by reacting tellurium powder with an n-butyl lithium solution to synthesize an n-butyl tellurium lithium solution, mixing the solution with chitosan, carrying out immersion treatment on the chitosan, and loading tellurium elements to obtain the tellurium-doped chitosan material.
In the invention, the molar ratio of the tellurium powder to the n-butyl lithium is 1: 1.
In the invention, the preparation steps of the n-butyl tellurium lithium solution are as follows: at the temperature of 0 +/-1 ℃, in an anhydrous and oxygen-free environment (glove box), stirring and mixing a 0.1mol/L n-butyl lithium cyclohexane solution with equal molar weight of tellurium powder, gradually heating to room temperature under stirring, and gradually disappearing the tellurium powder to obtain an n-butyl tellurium lithium solution.
In the invention, the n-butyl tellurium lithium solution is diluted by 20 times, added with chitosan to be soaked for 24 hours, filtered and washed to obtain the tellurium-doped chitosan material.
In the invention, the mass ratio of the tellurium powder to the chitosan is 0.01-0.2%: 1, wherein 0.1%: 1. at this ratio, tellurium can be utilized to the maximum extent, and the antibacterial activity of the material is relatively high.
In the invention, the tellurium-doped chitosan material has a tellurium mass content of 0.0011-0.016%, preferably 0.0072%. The material has the highest antibacterial activity at this tellurium content.
The tellurium-doped chitosan material is applied as an antibacterial material.
In the invention, the material can be sterilized under the drive of mild low-energy light (such as red light), and is expected to be used for manufacturing some antibacterial materials.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a brand-new tellurium-doped chitosan material. The material has simple preparation method, can be sterilized under the drive of mild low-energy light (such as red light), and has low toxicity.
Detailed Description
The following examples illustrate the invention in more detail, but do not limit the invention further.
In the invention, a new tellurium-doped chitosan material is designed. The material makes full use of the brittle and breakable property of tellurium chemical bonds, can generate active catalytic species under the drive of low-energy light, and catalyzes oxygen in air to oxidize organic molecules, thereby playing a role in sterilization.
Example 1
Material synthesis: in a glove box, 10mL of a 0.1mol/L n-butyllithium cyclohexane solution was injected into a 25mL round-bottomed flask containing 0.1276 g (i.e., 1mmol) of tellurium powder and a magnetic stirrer at a temperature of 0. + -. 1 ℃ under anhydrous and oxygen-free conditions. Magnetically stirring, stopping freezing until the temperature is raised to room temperature, transferring the obtained n-butyl tellurium lithium solution into a 1L beaker after tellurium powder gradually disappears, adding anhydrous cyclohexane to dilute the solution to 200mL, adding 127.6 g of chitosan (namely the mass of tellurium is 0.1 percent of that of the chitosan), soaking the solution for 24 hours, filtering the solution, washing the chitosan with anhydrous cyclohexane, and drying the chitosan in vacuum to obtain the tellurium-doped chitosan material. The mass content of tellurium in the material is 0.0072% as measured by inductively coupled plasma mass spectrometry, which indicates that 7.2% of tellurium in the used tellurium powder is loaded on chitosan.
Antibacterial activity test: the antibacterial activity test was performed under 5W LED red light irradiation (16 cm distance of light source from the experimental apparatus). The method comprises the following steps: research on tellurium-doped chitosan on gram-positive bacteria (staphylococcus aureus) through oscillation method bacteriostasis rate test experimentATCC 29213, Shanghai Lu Microscience Co., Ltd.) and gram-negative bacteria (Escherichia coli, ATCC 8099, Shanghai Lu Microscience Co., Ltd.). Accurately pipetting 5mL with a pipette at a concentration of about 105The cfu/mL bacterial solution was placed in a conical flask containing 70mL of PBS buffer solution, and then about (1X 2) cm2The tellurium-doped chitosan was spread therein (thickness about 0.5mm), and cultured in a constant temperature shaker for 18 hours, wherein the culture temperature was 37 ℃ and the rotation speed was constantly 200 rpm/min. After the culture is finished, sequentially diluting PBS buffer solution containing bacteria by a concentration gradient of 10 times, uniformly coating 5 mu L of PBS buffer solution on a solid culture medium, and culturing for 18h at a constant temperature of 37 ℃ in a constant-temperature incubator; after the culture is finished, calculating the viable count of each sample by using a plate counting method, repeating the experiment for three times, and taking an average value. The antibacterial effect determines the inhibition degree of bacteria, the viable count of the uncoated tellurium-doped chitosan is taken as a reference standard, and the calculation formula of the antibacterial rate is as follows:
Bacterial Inhibition％＝[(A-B)/A]×100％
in the above formula, a and B are the numbers of colonies of uncoated and coated new material tellurium-doped chitosan, respectively.
The bacteriostatic rates of the material on staphylococcus aureus (s. aureus) and escherichia coli (e. coli) were measured to be 96.43% and 94.28%, respectively. Acute toxicity test shows that the material has LD effect on mice50>5000mg/kg, which belongs to actual nontoxic materials (national committee for health and family planning of the people's republic of China, national standard of the people's republic of China, GB15193.3-2014, acute oral toxicity test of national standard for food safety, 2014).
Example 2
The other conditions are the same as example 1, related materials are synthesized by adopting different mass ratios of tellurium to chitosan, and the test is carried out, and the experimental results are shown in table 1.
Table 1 related materials testing synthesized with different tellurium to chitosan mass ratios
From the above results, it is understood that when 0.1% by mass of tellurium to chitosan is used, the content of tellurium in the material is 0.0072%, the antibacterial activity is excellent, and below this content, the antibacterial activity is remarkably decreased. But the antibacterial activity is not obviously improved by increasing the content of tellurium, and the best effect is achieved when the mass ratio of tellurium to chitosan is 0.1 percent in view of cost. When a lower amount of tellurium is used, the utilization rate of tellurium (namely the ratio of tellurium transferred from tellurium powder to materials) is higher, and after the mass ratio of tellurium to chitosan reaches 0.1%, the utilization rate of tellurium floats between 7.0% and 8.0% along with the further increase of the usage amount of tellurium. The chitosan has certain antibacterial property, under the test condition, the antibacterial rate of the chitosan to the two bacteria is 26.11 percent and 23.13 percent, which are obviously lower than the effect after tellurium doping, and the significant improvement of tellurium doping on the antibacterial activity of the material under the test condition (namely low-energy light irradiation) is fully demonstrated.
Example 3
The antibacterial effect of the material under different illumination conditions was tested under the same conditions as in example 1, and the results are shown in Table 2.
TABLE 2 examination of the antibacterial Effect of the materials under different illumination conditions
From the above results, it can be seen that the light irradiation can promote the antibacterial property of the material, which is consistent with the effect predicted by our theoretical analysis. The antimicrobial activity was maintained at 70% or more (number 2) even when the input power of the light irradiation energy was reduced. If white light and blue light with higher energy are used, the antibacterial rate can still be kept around 90 percent even if the power of the light source is reduced (serial numbers 3 and 4). Under the condition of no light, the antibacterial activity of the material is low, so that the importance of the antibacterial property of the material by light irradiation is reflected (serial number 5).
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any person skilled in the art can make any simple modification, equivalent replacement, and improvement on the above embodiment without departing from the technical spirit of the present invention, and still fall within the protection scope of the technical solution of the present invention.
Claims (11)
1. A tellurium-doped chitosan material is characterized in that the tellurium-doped chitosan material has a tellurium mass content of 0.0011-0.016%;
the preparation method comprises the following steps:
reacting tellurium powder with an n-butyl lithium solution to synthesize an n-butyl tellurium lithium solution, mixing the solution with chitosan, and carrying out immersion treatment on the chitosan to load tellurium element to obtain the tellurium-doped chitosan material.
2. The tellurium-doped chitosan material of claim 1, wherein the tellurium content is 0.0072% by mass.
3. The preparation method of the tellurium-doped chitosan material as claimed in claim 1 or 2, characterized in that tellurium powder is reacted with n-butyl lithium solution to synthesize n-butyl tellurium lithium solution, the solution is mixed with chitosan, the chitosan is dipped and treated, tellurium element is loaded, and the tellurium-doped chitosan material is obtained.
4. The method of claim 3, wherein the molar ratio of tellurium powder to n-butyllithium is 1: 1.
5. The method of claim 3, wherein the n-butyl tellurium lithium solution is prepared by the steps of: at the temperature of 0 +/-1 ℃, in an anhydrous and oxygen-free environment, stirring and mixing a cyclohexane solution of 0.1mol/L n-butyl lithium with tellurium powder in an equal molar amount, gradually heating to room temperature under stirring, and gradually disappearing the tellurium powder to obtain an n-butyl tellurium lithium solution.
6. The method as claimed in claim 3, wherein the tellurium-doped chitosan material is obtained by diluting the n-butyl tellurium lithium solution by 20 times, mixing the solution with chitosan, soaking for 24 hours, and carrying tellurium element by dipping treatment of the chitosan.
7. The method as claimed in claim 3, wherein the mass ratio of tellurium powder to chitosan is in the range of 0.01% to 0.2%: 1.
8. The method of claim 3, wherein the mass ratio of tellurium powder to chitosan is 0.1%: 1.
9. use of a tellurium-doped chitosan material of claim 1 or 2 as an antibacterial material.
10. The use of claim 9, wherein the material is sterilizable under low-energy light conditions.
11. The use of claim 9, wherein said bacteria comprise gram positive and gram negative bacteria.
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Citations (5)
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| CN102702240A (en) * | 2012-05-15 | 2012-10-03 | 玉林师范学院 | Organic hybridized telluride having photocatalytic performance and preparation thereof |
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Patent Citations (5)
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| CN102702240A (en) * | 2012-05-15 | 2012-10-03 | 玉林师范学院 | Organic hybridized telluride having photocatalytic performance and preparation thereof |
| CN103880084A (en) * | 2014-03-14 | 2014-06-25 | 南京航空航天大学 | Method of preparing superfine monolayer transition metal compound quantum dot solution |
| CN108191618A (en) * | 2018-01-16 | 2018-06-22 | 扬州大学 | A kind of method by tellurium catalytic oxime removal |
| CN108812694A (en) * | 2018-09-07 | 2018-11-16 | 江南大学 | A kind of nano-disinfection method for Gram-negative bacteria |
| CN111186822A (en) * | 2018-11-15 | 2020-05-22 | 南京理工大学 | Preparation method of tellurium nanoparticles |
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