A preparation method and application of norfloxacin test paper

Abstract

The invention discloses a preparation method and application of a norfloxacin test paper, belonging to the field of identification and detection technology, comprising the following steps: weighing five-membered cucurbitacin or cucurbituril [5], phenyl-4-butylamine, the molar ratio of which is 1:4, dissolving the five-membered cucurbitacin or cucurbituril [5] in water, heating and stirring to obtain a five-membered cucurbitacin or cucurbituril [5] solution, dissolving the phenyl-4-butylamine in water, stirring to obtain a phenyl-4-butylamine solution after adding hydrochloric acid to the phenyl-4-butylamine solution, mixing the five-membered cucurbitacin or cucurbituril [5] solution and the phenyl-4-butylamine solution, and obtaining a cucurbitacin-based supramolecular organic framework material after being statically volatilized, dissolving the cucurbitacin-based supramolecular organic framework material in water to obtain a cucurbitacin-based supramolecular organic framework material aqueous solution, taking filter paper and soaking it in the cucurbitacin-based supramolecular organic framework material aqueous solution, and taking out and drying after soaking. The cucurbitacin-based supramolecular organic framework material of the present invention can be used to detect norfloxacin.

Description

Technical Field

[0001] The invention belongs to the technical field of identification and detection, and specifically relates to a preparation method and application of a norfloxacin test paper. Background Art

[0002] As a quinolone antibiotic, norfloxacin (NFX) has the advantages of broad-spectrum antibacterial activity, strong antibacterial activity, high safety, and low price. It is widely used in the prevention and treatment of bacterial infections in the medical field and animal diseases in the breeding field. However, due to its non-biodegradability, NFX is prone to cumulative effects after entering the environment. In addition, its serious abuse leads to serious drug residues, which poses a serious threat to the ecological environment and human health. Studies have shown that excessive intake of NFX or long-term intake of foods containing low concentrations of NFX can induce drug resistance in pathogens, promote the production of "super-resistant bacteria", make antibiotics ineffective, and easily induce symptoms such as diarrhea, nausea, vomiting, dizziness, headache, and drowsiness, and even seriously affect children's growth and development. Therefore, it is very necessary to develop a technology for rapid, simple, and accurate detection of NFX. Although a variety of technologies have been reported to be used for the detection of NFX, such as liquid chromatography-mass spectrometry (LCMS), high performance liquid chromatography (HPLC), micellar electrokinetic capillary chromatography (MECC), surface enhanced Raman spectroscopy (SERS), etc., these detection technologies often require large-scale instruments and equipment, and are expensive, complex to operate, require cumbersome sample preparation, and slow to test, which greatly limits their practical applications. Summary of the invention

[0003] In view of the deficiencies in the prior art, the object of the present invention is to provide a preparation method and application of a norfloxacin test paper.

[0004] The purpose of the present invention can be achieved through the following technical solutions:

[0005] A method for preparing a test paper comprises the following steps:

[0006] Weigh five-membered cucurbitacin or cucurbituril [5] and phenyl-4-butylamine respectively at a molar ratio of 1:4, dissolve the five-membered cucurbitacin or cucurbituril [5] in water, heat and stir to obtain a five-membered cucurbitacin or cucurbituril [5] solution, dissolve phenyl-4-butylamine in water, add hydrochloric acid to the phenyl-4-butylamine solution and stir to obtain a phenyl-4-butylamine solution, mix the five-membered cucurbitacin or cucurbituril [5] solution and the phenyl-4-butylamine solution, and allow to volatilize to obtain a cucurbitacin-based supramolecular organic framework material;

[0007] The cucurbitacin-based supramolecular organic framework material is dissolved in water to obtain a cucurbitacin-based supramolecular organic framework material aqueous solution, and a filter paper is soaked in the cucurbitacin-based supramolecular organic framework material aqueous solution, and then taken out and dried after soaking.

[0008] Furthermore, during the preparation of the five-membered cucurbitacin or cucurbituril [5] solution, the heating temperature is 50°C to 80°C, and the five-membered cucurbitacin or cucurbituril [5] solution is 10 mg·mL -1 .

[0009] Furthermore, the specific preparation process of the phenyl-4-butylamine solution is to pipette 6 μL of phenyl-4-butylamine ligand into 1 mL of water, and then add 500 μL of 1 mol·L -1 HCl solution.

[0010] Furthermore, the five-membered cucurbitacin or cucurbituril [5] solution and the phenyl-4-butylamine solution are mixed so that both solutions are clear and transparent before mixing.

[0011] Furthermore, the aqueous solution of the cucurbitacin-based supramolecular organic framework material is 30 mL 1 mg·mL -1 Solution.

[0012] Furthermore, the filter paper needs to be completely immersed during the soaking process.

[0013] Furthermore, the test paper after immersion is dried in a vacuum drying oven at 80° C. for 6 hours.

[0014] Beneficial effects of the present invention:

[0015] The invention discloses a preparation method and application of a norfloxacin test paper. The "counter cation" of the protonated 4-phenylbutylamine ligand is used to balance the charge of the system, and the "hydrogen bond receptor" of the amino group is used to play a "bridging" role. A new type of cucurbitacin-based supramolecular organic framework material is designed and synthesized, and a portable test paper for detecting norfloxacin is prepared using the material.

[0016] The preparation method of a cucurbitacin-based supramolecular organic framework material provided by the present invention has the characteristics of simple operation, low energy consumption, short time, low cost, etc. The test paper prepared by the method can highly efficiently identify norfloxacin. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0018] Figure 1 is a crystal structure diagram of the cucurbitacin-based supramolecular framework material of the present invention;

[0019] Figure 2is a SEM image of the cucurbitacin-based supramolecular framework material of the present invention;

[0020] Figure 3 The test paper contaminated with NFX in the present invention has obvious blue fluorescence under 254nm ultraviolet light;

[0021] Figure 4 It is the fluorescence qualitative titration result of the cucurbitacin-based supramolecular organic framework material of the present invention for detecting different antibiotics;

[0022] Figure 5 This is a fluorescence titration spectrum of the cucurbitacin-based supramolecular organic framework material of the present invention for detecting norfloxacin. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] A method for preparing cucurbitacin-based supramolecular organic framework material

[0025] The preparation method of the cucurbitacin-based supramolecular organic framework material of this embodiment comprises the following steps:

[0026] Step 1, five-membered cucurbituril or cucurbituril [5] and phenyl-4-butylamine are mixed in a molar ratio of 1:4 and the volume and mass are calculated respectively;

[0027] Step 2: dissolving the five-membered cucurbitacin or cucurbituril [5] in an appropriate amount of water, heating, and stirring with a strong magnetic force;

[0028] Step 3: Add the pre-calculated ligand into an appropriate amount of water, add an appropriate amount of hydrochloric acid to protonate it, and stir with strong magnetic force;

[0029] Step 4: After both become clear and transparent solutions, mix them evenly at room temperature, place them in a fume hood and let them evaporate for a period of time to obtain a cucurbitacin-based supramolecular organic framework material, wherein the cucurbitacin-based supramolecular organic framework material is in the shape of colorless block crystals.

[0030] Step 5: Add the cucurbitacin-based supramolecular organic framework material obtained above into deionized water and dissolve it by ultrasonic oscillation.

[0031] Step 6: Soak the cut laboratory filter paper into the aqueous solution of the cucurbitacin-based supramolecular organic framework material, remove it and dry it after a period of time.

[0032] In step 2, the mixture is heated to 50°C to 80°C and stirred with strong magnetic force to dissolve the cucurbitacin ring, and then prepared into 10 mg mL -1 Q[5] solution, in step 3, pipette (6 μL, 0.038 mmol) of phenyl-4-butylamine ligand into 1 mL of water, and add 500 μL of 1 mol·L -1 HCl solution. In step 4, both solutions must be completely clear and transparent. In step 5, the aqueous solution of the cucurbitacin-based supramolecular organic framework material is prepared into 30 mL of 1 mg·mL -1 The solution was placed in a 50 mL centrifuge tube. The filter paper in step 6 was completely immersed in the aqueous solution of the cucurbitacin-based supramolecular organic framework material for 24 hours. The test paper taken out in step 6 was dried in a vacuum drying oven at 80°C for 6 hours. The detailed analysis of its crystal structure is as follows Figure 1 Scanning electron microscopy (SEM) of solid samples Figure 2 .

[0033] The obtained cucurbitacin-based supramolecular organic framework material is added to deionized water and ultrasonically oscillated to dissolve it. Cut laboratory filter paper is soaked in the aqueous solution of cucurbitacin-based supramolecular organic framework material, and after a period of time, it is removed and dried to prepare a test paper. Different solutions are added to the test paper. When the solution contains norfloxacin, the test paper will emit obvious blue fluorescence under the irradiation of a 254nm ultraviolet lamp, such as Figure 3 .

[0034] Figure 4 , Figure 5 This is the fluorescence detection of different antibiotics by the cucurbitacin-based supramolecular organic framework material. As can be seen from the figure, after the addition of norfloxacin, the fluorescence curve and intensity of the cucurbitacin-based supramolecular organic framework material changed significantly.

[0035] Table 1 Crystal structure parameters of the cucurbitacin-based supramolecular organic framework material of the present invention

[0036]

[0037] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0038] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments, and the above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, and these changes and improvements all fall within the scope of the present invention to be protected.

Claims

1. A method for preparing a test paper, characterized in that: The following steps are involved: Weigh five-membered cucurbitacin or cucurbituril [5] and phenyl-4-butylamine respectively in a molar ratio of 1:4, dissolve the five-membered cucurbitacin or cucurbituril [5] in water, heat and stir to obtain a five-membered cucurbitacin or cucurbituril [5] solution, dissolve phenyl-4-butylamine in water, add hydrochloric acid to the phenyl-4-butylamine solution and stir to obtain a phenyl-4-butylamine solution, mix the five-membered cucurbitacin or cucurbituril [5] solution and the phenyl-4-butylamine solution, and allow to volatilize to obtain a cucurbitacin-based supramolecular organic framework material; The cucurbitacin-based supramolecular organic framework material is dissolved in water to obtain a cucurbitacin-based supramolecular organic framework material aqueous solution, and a filter paper is soaked in the cucurbitacin-based supramolecular organic framework material aqueous solution, and then taken out and dried after soaking.

2. The method for preparing a test paper according to claim 1, characterized in that: During the preparation of the five-membered cucurbitacin or cucurbituril [5] solution, the heating temperature is 50°C to 80°C, and the five-membered cucurbitacin or cucurbituril [5] solution is 10 mg·mL -1 .

3. The method for preparing a test paper according to claim 1, characterized in that: The specific preparation process of the phenyl-4-butylamine solution is to pipette 6 μL of phenyl-4-butylamine ligand into 1 mL of water, and then add 500 μL of 1 mol·L -1 HCl solution.

4. The method for preparing a test paper according to claim 1, characterized in that: The five-membered cucurbitacin or cucurbituril [5] solution and the phenyl-4-butylamine solution are mixed and both solutions are in a clear and transparent state before mixing.

5. The method for preparing a test paper according to claim 1, characterized in that: The aqueous solution of the cucurbitacin-based supramolecular organic framework material is 30 mL 1 mg·mL -1 Solution.

6. The method for preparing a test paper according to claim 1, characterized in that: The filter paper needs to be completely soaked during the soaking process.

7. The method for preparing a test paper according to claim 1, characterized in that: The test paper after immersion was dried in a vacuum drying oven at 80° C. for 6 hours.

8. Use of the test paper prepared by the method for preparing a test paper according to any one of claims 1 to 7 in the detection of norfloxacin.

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