Multifunctional effervescent tablet as well as preparation method and application thereof

Through the use of multifunctional effervescent tablets, combined with effervescent assisted derivatization and magnetic solid-phase extraction technology, the integrated operation of sample pretreatment is achieved, the complex and time-consuming operation in the existing technology is solved, the detection efficiency and sensitivity are improved, and it is suitable for the detection of trace targets in complex water samples.

CN120064525APending Publication Date: 2025-05-30ZHENGZHOU UNIV
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Patent Information

Application Number
CN202510199262.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-24
Publication Date
2025-05-30

AI Technical Summary

Technical Problem

The existing sample pretreatment methods are complex, time-consuming, and difficult to effectively process target analytes with strong polarity, low thermal stability or weak detection signal response.

Method used

Using multifunctional effervescent tablets, the integrated operation of derivatization, enrichment, and solid-liquid separation is achieved through the organic combination of effervescent assisted derivatization and magnetic solid-phase extraction technology. Effervescent tablets are composed of effervescent precursors, magnetic materials, adsorbents and derivatization reagents. Through one-step tableting molding, they can quickly disintegrate in the aqueous medium and automatically release functional components, achieving efficient derivatization and enrichment of target analytes.

Benefits of technology

The sample pre-processing process is simplified, the detection efficiency is improved, the operation complexity and time cost is significantly reduced, the detection convenience and repetition are improved, and the trace targets in complex water samples can be effectively processed.

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Abstract

The invention belongs to the technical field of analysis detection and sample pretreatment, and particularly relates to a multifunctional effervescent tablet as well as a preparation method and application thereof. According to the preparation method of the multifunctional effervescent tablet, the effervescent precursor, the magnetic material, the adsorbent and the derivatization reagent are combined and subjected to one-step tabletting forming, and when the prepared multifunctional effervescent tablet is used for target analyte detection, multifunctional integration of automatic effervescent mixing, derivatization reaction of target analytes, magnetic solid-phase extraction and the like can be achieved; according to the method, the efficiency, convenience and sensitivity of sample pretreatment can be remarkably improved, the application range of an effervescence-assisted microextraction technology is expanded, meanwhile, a convenient and efficient new strategy can be provided for the sample pretreatment technology, and the method is very suitable for detection of trace target analytes in a complex water sample.
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Description

Technical Field

[0001] The present invention belongs to the technical field of analytical detection and sample pretreatment, and particularly relates to a multifunctional effervescent tablet, a preparation method thereof and an application thereof. Background Art

[0002] In the field of modern analytical detection, sample pretreatment is a key step affecting detection sensitivity, selectivity and accuracy. Traditional sample pretreatment methods mainly include liquid-liquid extraction (LLE), solid-phase extraction (SPE), magnetic solid-phase extraction (MSPE) and derivatization reactions, etc. However, these methods often involve multiple cumbersome operation steps, such as solvent evaporation, shaking, centrifugation, filtration and separate addition of derivatization reagents, which are not only time-consuming and laborious, but also may lead to the accumulation of experimental errors. In addition, some target analytes need to be derivatized to improve chromatographic separation effect or detection sensitivity due to strong polarity, low thermal stability or weak detection signal response, while traditional derivatization reactions usually require additional heating or stirring, further increasing the complexity of the experiment.

[0003] In recent years, the effervescence-assisted microextraction (EAME) technique, as a new sample pretreatment method, has received wide attention. The effervescence technique is based on an acid-base reaction to generate CO 2 to promote the rapid release of components. The generation of bubbles forms a violent disturbance in the solution, enhancing the dispersion of the extractant or adsorbent in the sample solution, thereby accelerating the extraction or adsorption process of the target analyte. This bubble-assisted dispersion mechanism effectively avoids the dependence on external equipment such as mechanical stirring or ultrasonic waves, reducing the operation cost and energy consumption. Usually, the effervescent agent consists of carbonate (such as sodium carbonate, sodium bicarbonate) and acid (such as sodium dihydrogen phosphate, tartaric acid, citric acid), and the two react in the aqueous phase to release carbon dioxide gas. The formation of bubbles not only helps the uniform dispersion of the adsorbent, but also significantly improves the mass transfer efficiency of the target substance, thereby enhancing the extraction performance.

[0004] At present, the EAME technique has evolved into various improved modes to adapt to different types of samples and analysis requirements, including liquid-liquid effervescence-assisted microextraction, solid-liquid effervescence-assisted microextraction and magnetic effervescence-assisted solid-phase microextraction, etc. However, most of the effervescent tablets used in the existing EAME techniques only play the role of promoting the effervescence reaction and dispersing the extractant or adsorbent. The same is true for most of the other related methods reported in the existing literature, which makes additional steps still required for sample pretreatment, such as the preparation of magnetic adsorbents, derivatization, etc., and there will still be problems such as cumbersome operation procedures, long time consumption and accumulation of experimental errors. Summary of the Invention

[0005] In order to overcome the deficiencies of the prior art, the object of the present invention is to provide a preparation method of a multifunctional effervescent tablet, which realizes the integrated operation of derivatization, enrichment, and solid-liquid separation through the organic combination of effervescent-assisted derivatization and magnetic solid-phase extraction technology, providing a new efficient, convenient, and stable strategy for the pretreatment of complex samples, and is very suitable for the rapid detection of trace target substances (ng / g, ng / mL) in complex water samples.

[0006] The object of the present invention is also to provide the multifunctional effervescent tablet prepared by the above preparation method and its application, as well as a method for detecting target analytes using the above multifunctional effervescent tablet.

[0007] To achieve the above object, in the first aspect of the present invention, a preparation method of a multifunctional effervescent tablet is provided, including the following steps: uniformly mixing an effervescent precursor, a magnetic material, an adsorbent, and a derivatization reagent, and then tabletting to obtain the multifunctional effervescent tablet.

[0008] As a preferred embodiment of the present invention, the effervescent precursor consists of an H + donor and a CO 2 donor; the H + donor is selected from one or more of sodium dihydrogen phosphate, citric acid, tartaric acid, ascorbic acid, ammonium bicarbonate, and sodium bisulfate; the CO 2 donor is selected from one or more of sodium carbonate, sodium bicarbonate, and calcium carbonate; the molar ratio of the H + donor to the CO 2 donor is (1-3):1. By controlling the molar ratio of the two, the disintegration rate can be ensured to be moderate.

[0009] As a preferred embodiment of the present invention, the magnetic material is one or more of Fe 3 O 4 nanoparticles, Fe 2 O 3 nanoparticles, CoFe 2 O 4 cobalt ferrite, NiFe 2 O 4 nickel ferrite, Fe 3 O 4 @SiO 2 magnetic silica.

[0010] As a preferred embodiment of the present invention, the adsorbent is one or more of hydroxylated multi-walled carbon nanotubes, graphene, polypyrrole, polyaniline, metal-organic framework materials, and covalent organic framework materials.

[0011] Derivatization reagents are used to enhance the signal response intensity of target analytes in instrumental detection. When selecting them, it is necessary to rely on the functional groups contained in the target analytes to ensure that the target analytes can undergo specific reactions with the derivatization reagents. As a preferred embodiment of the present invention, the derivatization reagent is selected from one of fluorescamine, 2,4-dinitrophenylhydrazine, and dansyl chloride.

[0012] By controlling the raw material ratio during the preparation of the effervescent tablets, the efficiency of the effervescent reaction and the synchronous progress of the derivatization reaction are ensured. As a preferred embodiment of the present invention, the mass ratio of the magnetic material, adsorbent, and derivatization reagent is (3-5):1:(0.5-2).

[0013] The preparation method of the multifunctional effervescent tablets provided by the present invention combines an effervescent precursor, a magnetic material, an adsorbent, and a derivatization reagent to form a tablet by one-step pressing. Among them, the effervescent precursor reacts rapidly in the aqueous phase to release CO 2 , forming a large number of bubbles, promoting solution mixing, and improving the extraction efficiency. The derivatization reagent released during the effervescent reaction can induce the derivatization reaction and improve the detection signal response of the analyte. At the same time, the magnetic material and the adsorbent self-assemble to form a magnetic adsorption material during the effervescent reaction, efficiently enriching the derivatization products of the analyte.

[0014] Therefore, the multifunctional effervescent tablets prepared by the present invention achieve the integration of multifunctions such as effervescent automatic mixing, derivatization reaction of target analytes, and magnetic solid-phase extraction. Compared with the traditional method, the effervescent tablets prepared by the present invention can quickly disintegrate in the aqueous medium, promote solution mixing through CO 2 , and can complete the enrichment and derivatization of target analytes without external stirring or shaking. At the same time, solid-liquid separation can be achieved by using an external magnet, greatly simplifying the traditional sample pretreatment process and improving the detection efficiency. Moreover, the preparation process of the effervescent tablets of the present invention is simple, flexible to use, does not require additional instruments during the derivatization extraction process, is convenient to carry and operate, significantly improves the applicability and convenience of analysis and detection, also improves the experimental efficiency and repeatability, and can provide a novel and convenient technical approach for sample pretreatment.

[0015] As a preferred embodiment of the present invention, the uniform mixing is carried out by grinding and mixing. The diameter of the multifunctional effervescent tablets is 5-20 mm, and the thickness is 1-10 mm. Further preferably, the diameter of the multifunctional effervescent tablets is 8-15 mm, and the thickness is 2-6 mm. More preferably, the diameter of the multifunctional effervescent tablets is 8 mm, and the thickness is 2 mm.

[0016] In the second aspect of the present invention, a multifunctional effervescent tablet prepared by the above preparation method is provided.

[0017] The multifunctional effervescent tablets of the present invention can automatically dissolve and release functional components in an aqueous medium, thereby realizing the efficient derivatization and enrichment of target analytes. In particular, by integrating the effervescent reaction, derivatization reaction, and magnetic solid-phase extraction, the multifunctional effervescent tablets can avoid complex operation steps in traditional methods, such as mechanical stirring, ultrasonic dispersion, centrifugal filtration, etc., greatly simplifying the sample pretreatment process and improving the detection efficiency.

[0018] By optimizing the composition design of the effervescent tablets, the present invention enables them to not only release CO 2 during the dissolution process to promote solution mixing, but also synchronously induce the derivatization reaction and form a magnetic adsorption material, thus completing derivatization and extraction in one step. Compared with traditional sample pretreatment techniques, this method combines the effervescent reaction, derivatization reaction, and magnetic adsorption technology, and through automatic dissolution and component release, realizes the efficient derivatization and enrichment of samples, significantly reducing the operation complexity and time cost, improving the convenience and repeatability of detection, and can be widely applied to the pretreatment processes in the fields of food safety detection, drug analysis, bioanalysis, environmental monitoring, etc. to improve the detection sensitivity and accuracy of analytes.

[0019] In a third aspect of the present invention, there is provided an application of the above-mentioned multifunctional effervescent tablets in the detection of target analytes; the target analytes are aldehyde compounds, ketone compounds, or amine compounds.

[0020] As a further preferred embodiment of the present invention, the target analyte is a sulfonamide compound. The sulfonamide compounds are selected from one or more of sulfaguanidine, sulfanilamide, sulfadiazine, sulfamethazine, sulfamonomethoxine, sulfamethoxypyridazine, sulfamethoxazole, sulfabenzamide, and sulfadimethoxine.

[0021] As a further preferred embodiment of the present invention, when the target analyte is a sulfonamide compound, the H + donor is sodium dihydrogen phosphate; the CO 2 donor is sodium carbonate; the magnetic material is Fe 3 O 4 nanoparticles; the adsorbent is hydroxylated multi-walled carbon nanotubes; the derivatization reagent is fluorescamine. The molar ratio of the H + donor to the CO 2 donor is 2:1; the mass ratio of the magnetic material, adsorbent, and derivatization reagent is 3:1:0.5. The multifunctional effervescent tablets prepared based on the above conditions can realize the high-sensitivity detection of various sulfonamide compounds in water samples.

[0022] In the fourth aspect of the present invention, a method for detecting a target analyte using the above multi-functional effervescent tablet is provided, including the following steps: adjusting the acidity of a sample solution containing the target analyte, then adding the multi-functional effervescent tablet, performing extraction derivatization treatment while realizing the effervescence reaction, further cleaning and desorbing the obtained derivatized product under the action of an external magnetic field, and then performing instrumental analysis on the obtained desorbed solution, thereby realizing the detection of the target analyte; wherein, the time of the effervescence reaction is 2 to 10 min.

[0023] In the above detection method of the present invention, the multi-functional effervescent tablet used can rapidly disintegrate in an aqueous medium and realize sample pretreatment through the following mechanism: the effervescence reaction releases CO 2 , promoting solution mixing; the derivatization reagent dissolves out, promoting the effervescence reaction and simultaneously performing a derivatization reaction; the magnetic material and the adsorbent self-assemble to form a magnetic adsorbent material to enrich the derivatized product of the target analyte.

[0024] As a preferred embodiment of the present invention, the adjustment of acidity treatment is to add a regulator for treatment. The regulator is one of sodium acetate, citric acid, and oxalic acid. The regulator is used to optimize the effervescent dissolution environment to promote the occurrence of the effervescence reaction and the efficient progress of the derivatization reaction. Those skilled in the art can conventionally select a buffer reagent suitable for the processes of analytical detection, effervescence, derivatization, and extraction as the regulator.

[0025] As a preferred embodiment of the present invention, the desorption is to perform desorption treatment on the derivatized product using a desorption solvent; the desorption solvent is one or more of acetonitrile, acetone, ethyl acetate, and methanol.

[0026] The present invention does not particularly limit the type of instrument used for instrumental analysis. Those skilled in the art can conventionally select an analytical instrument matching the derivatized product. As a preferred embodiment of the present invention, the instrument used for instrumental analysis is one of an ultraviolet-visible spectrophotometer (UV-Vis), high performance liquid chromatography (HPLC), gas chromatography-mass spectrometry (GC-MS), and liquid chromatography-mass spectrometry (LC-MS).

[0027] Compared with the existing sample pretreatment methods, the multi-functional effervescent tablet and the detection method of the present invention have the following advantages:

[0028] (1) Simple operation: The effervescent tablet can automatically dissolve in an aqueous medium and release functional components, without additional stirring, shaking, or heating processes, which is beneficial to reducing experimental errors and improving repeatability.

[0029] (2) Integrated integration: Integrating the effervescence reaction, derivatization, and magnetic solid phase extraction functions into the same tablet, completing the enrichment and derivatization of the analyte in one step, and improving the detection efficiency.

[0030] (3) Improving detection sensitivity: The derivatization reagent is automatically released during the effervescence process, enhancing the detection signal response of the target analyte; moreover, the self-assembly enrichment of the magnetic adsorption material increases the concentration of the target analyte.

[0031] (4) Strong adjustability: The composition of the effervescent tablet can be adjusted according to different analysis requirements, such as adding different derivatization reagents or adsorption materials to adapt to different sample types and different kinds of target analytes.

[0032] (5) Wide applicability: It is applicable to the analysis and detection of food, drugs, biological fluids, and environmental samples, especially suitable for the pretreatment of complex matrix samples, reducing matrix interference and improving the accuracy of detecting target analytes at the nanogram level.

[0033] (6) Convenient for carrying and storage: The tablet form is stable, with a small volume, making it easy to carry and store. It is more operable than traditional liquid reagents and is suitable for on-site rapid detection and portable analysis.

[0034] In summary, the present invention provides a preparation method of a multifunctional effervescent tablet and its application in analysis and detection, significantly improving the efficiency, convenience, and sensitivity of sample pretreatment, expanding the application scope of the effervescence-assisted microextraction technology, providing a convenient and efficient new strategy for sample pretreatment technology, and being very suitable for the detection of trace target analytes such as sulfonamides in complex water samples. Brief Description of the Drawings

[0035] Figure 1 It is a flow chart of the preparation method of the multifunctional effervescent tablet in Example 1 of the present invention and the detection of the target analyte.

[0036] Figure 2 It is a liquid chromatogram of the detection of nine sulfonamide compounds in water samples using the multifunctional effervescent tablet and detection method in Example 1 of the present invention. Detailed Description of the Specific Embodiment

[0037] In order to more clearly understand the above-mentioned objects, features, and advantages of the present invention, the present invention will be further described in detail below in conjunction with specific embodiments. It should be noted that, without conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other. Among them, the hydroxylated multi-walled carbon nanotubes involved in the following embodiments are from the Shanghai Aladdin brand; the iron oxide nanoparticles are from the Xianfeng Nano brand. Other raw materials and preparation methods, unless otherwise specified, are conventional materials and technologies in the art.

[0038] In the following embodiments of the present invention, the detection of nine sulfonamide compounds in water samples is taken as an example to illustrate the preparation method and application mode of the multifunctional effervescent tablets of the present invention. In other embodiments, the target analyte to be detected can also be trace analytes that need to be efficiently enriched in other complex matrices, including but not limited to various aldehyde compounds, ketone compounds, or amine compounds, etc. As long as the selected target is within the application concept of the multifunctional effervescent tablets of the present invention, the detection effect of the present invention can also be achieved. Therefore, the present invention does not particularly limit the types of target analytes.

[0039] Example 1

[0040] In this example, the detection of nine sulfonamide compounds in water samples is taken as an example to illustrate the preparation method and application mode of the multifunctional effervescent tablets of the present invention. Specifically, this example provides a multifunctional effervescent tablet, which efficiently derivatizes and enriches nine sulfonamide target substances in water samples, and uses high-performance liquid chromatography-fluorescence detection (HPLC-FLD) for quantitative analysis. Among them, the nine sulfonamide target substances are sulfaguanidine (SGN), sulfonamide (SA), sulfadiazine (SDZ), sulfamethoxazole (SMZ), sulfamonomethoxine (SMM), sulfamethazine (SMD), sulfamethoxazole (SMX), sulfabenzamide (SB), and sulfamethoxazole (SDM).

[0041] The flow schematic diagram of the preparation method and detection process of the multifunctional effervescent tablet is as Figure 1 shown, and specifically includes the following steps:

[0042] (1) Preparation of the multifunctional effervescent tablet: Mix the pre-effervescent agent, magnetic material, adsorbent, and derivatization reagent evenly; among them, the pre-effervescent agent is composed of sodium dihydrogen phosphate (NaH 2 PO 4 , 83.24 mg) and anhydrous sodium carbonate (Na 2 CO 3 , 36.76 mg) mixed in a molar ratio of 2:1. The magnetic material is magnetite nanoparticles (Fe 3 O 4, 6 mg), the adsorbent is hydroxylated multi-walled carbon nanotubes (MWCNTs-OH, 2 mg), the magnetic material and the adsorbent are proportioned by a mass ratio of 3:1, and the derivatization reagent is fluorescamine (1 mg). The above components are mixed in a mortar and ground thoroughly, and then the uniformly mixed powder is pressed into a multifunctional effervescent tablet with a diameter of 8 mm and a thickness of 2 mm using a powder press.

[0043] (2) Derivatization extraction process: Add 2 mL of sulfonamide sample solution (an aqueous solution prepared from nine sulfonamide compound standards, and the concentration of each sulfonamide target is 20 ng / mL) to a centrifuge tube, and then add 200 μL of sodium acetate buffer solution (50 mM, pH 3.5) to adjust the acidity of the solution; then place a multifunctional effervescent tablet prepared in step (1) into the centrifuge tube containing the sulfonamide sample solution, and an effervescence reaction will immediately occur and a large amount of CO 2 bubbles will be generated rapidly, promoting the mixing of the solution and accelerating the release of the components. At the same time, the derivatization reagent fluorescamine dissolves rapidly and undergoes a chemical derivatization reaction with the sulfonamide target analyte to form a derivatization product. After 2 minutes of starting the effervescence process, the derivatization reaction is basically completed. Meanwhile, the magnetic material (magnetite nanoparticles) released during the effervescence process self-assembles with the adsorbent (hydroxylated multi-walled carbon nanotubes) to form a magnetic adsorbent material, which specifically adsorbs the derivatization product of fluorescamine and sulfonamides. Subsequently, an external magnetic field is applied at the bottom of the centrifuge tube, so that the magnetic adsorbent adsorbed with the derivatization product is separated from the sample solution by magnetic separation. After discarding the supernatant, add 500 μL of pure water to wash the magnetic adsorbent for 0.5 minutes and remove the washing solution. Then add 250 μL of acetone as the desorbing solution and vortex mix for 2 minutes to elute the derivatization product on the adsorbent, and collect the desorbing solution. After the desorbing solution is filtered through a 0.22 μm filter membrane, a sample is taken for liquid chromatography analysis.

[0044] (3) Instrumental analysis and detection: To achieve the qualitative and quantitative analysis of sulfonamide targets (SAs) in water samples, high performance liquid chromatography - fluorescence detector (HPLC - FLD) was used for detection. The analysis conditions of HPLC - FLD were as follows: A Waters (model ACQUITY - e2695) high performance liquid chromatography system equipped with a fluorescence detector was used to analyze SAs. An Agilent 5TC - C18 chromatographic column (250×4.6 mm, 5 μm) was used for liquid chromatography separation. The mobile phase consisted of: (A) aqueous solution containing 0.1% formic acid and (B) acetonitrile aqueous solution containing 0.1% formic acid, with a flow rate of 1.0 mL / min. Isocratic elution: 0 - 30 min, 60% A, 40% B (isothermal). The excitation wavelength of the fluorescence detector (FLD) was 395 nm, and the emission wavelength was 491 nm. The column temperature was maintained at 30 °C. The temperature of the autosampler was 4 °C, and the injection volume was 20 μL. Each analysis run lasted for a total of 30 min. Waters Empower 3.1 software was used for data acquisition and processing.

[0045] In this example, by derivatizing, extracting, and determining the sulfonamide sample solution, the effectiveness of the method of applying the multifunctional effervescent tablets of the present invention to compound detection was investigated. To further confirm the technical effects of the present invention, the detection results of Example 1 of the present invention were compared with the test results of the control group and the blank group.

[0046] Among them, in the control group experiment, only the above - mentioned same sulfonamide sample solution (20 ng / mL) was derivatized, and the multifunctional effervescent tablets were not used for extraction and enrichment. The specific operation was as follows: Take 2 mL of sulfonamide sample solution (an aqueous solution prepared with nine sulfonamide compound standards, and the concentration of each sulfonamide target was 20 ng / mL) in a 2 mL centrifuge tube, add 200 μL of sodium acetate buffer solution (50 mM, pH 3.5) to adjust the acidity of the solution to promote the derivatization reaction. Subsequently, add 100 μL of fluorescamine reagent with a concentration of 10 mg / mL (dissolved in acetonitrile), mix well and let it stand in the dark at room temperature for 5 minutes to ensure that the sulfonamide compounds fully undergo derivatization reaction with fluorescamine to form stable derivatization products. After the reaction was completed, add 500 μL of pure water to the centrifuge tube, vortex for 10 s to mix evenly, take 250 μL of the reaction solution, filter it through a 0.22 μm filter membrane, and take a 20 μL sample and directly inject it into a high performance liquid chromatography - fluorescence detector (HPLC - FLD) for analysis and detection. The HPLC - FLD conditions were the same as those in Example 1. In the blank group experiment, the multifunctional effervescent tablets prepared in Example 1 of the present invention were used for sample pretreatment of a blank water sample without the target, and then chromatographic analysis was carried out under the chromatographic analysis conditions of Example 1.

[0047] The liquid chromatography detection results are as Figure 2as shown in the figure. Among them, Figure 2 In Figure 2 , chromatogram a is the chromatogram obtained by performing sample pretreatment on the sulfonamide sample solution with the multifunctional effervescent tablet prepared in Example 1 of the present invention and then performing chromatographic analysis; chromatogram b is the chromatogram obtained by only derivatizing the sulfonamide sample solution of the control group and then performing chromatographic analysis, which is used as a reference standard; chromatogram c is the chromatogram obtained by performing sample pretreatment on the blank water sample with the multifunctional effervescent tablet prepared in Example 1 of the present invention and then performing chromatographic analysis.

[0048] From Figure 2 the chromatographic results, it can be seen that after the treatment in Example 1 of the present invention, the chromatographic peaks in chromatogram a correspond one by one to the reference standard in chromatogram b, indicating that the derivatization reaction is successful, and the significantly enhanced signal intensity in chromatogram a compared to chromatogram b indicates that the target derivatization product is effectively enriched. Moreover, no chromatographic peaks corresponding to the target analyte derivatives appear in chromatogram c, indicating that there is no obvious matrix interference or background noise in this method.

[0049] The above experimental results show that the multifunctional effervescent tablet of the present invention can effectively promote the derivatization reaction of the target analyte, and through magnetic adsorption enrichment, improve the detection sensitivity, providing an efficient and convenient sample pretreatment strategy for the rapid detection of trace target substances (such as sulfonamide compounds) in complex water samples.

[0050] In summary, the main advantages of the multifunctional effervescent tablet and the detection method provided by the method of the present invention are reflected in the following aspects: First, the automatic release characteristic of the effervescent tablet makes the sample pretreatment more convenient. Without additional stirring or shaking, the solution mixing and derivatization reaction can be completed, reducing the operation error and experimental steps; Second, the derivatization reagent and the adsorbent are released synchronously during the effervescent process, enabling the derivatization and the enrichment of the target analyte to be carried out simultaneously, improving the detection efficiency; Third, the magnetic adsorbent is formed in situ in the solution, achieving efficient capture of the target analyte and rapid separation by applying an external magnet, avoiding the centrifugation or filtration steps. In particular, the HPLC-FLD analysis results show that the method of the present invention has good specificity and high sensitivity, and is suitable for the detection of target compounds at the nanogram level (ng / g, ng / mL) in complex water samples.

[0051] Therefore, taking the detection of sulfonamide compounds as an example, the present invention proves the application value of the multifunctional effervescent tablet in the analysis of trace sulfonamide compounds in water samples. The detection method of the present invention realizes the integrated operation of derivatization, enrichment, and solid-liquid separation through the organic combination of effervescent-assisted derivatization and magnetic solid-phase extraction technology, providing an efficient, convenient, and stable new strategy for complex sample pretreatment, and having a broad application prospect in sample pretreatment.

[0052] The above embodiments are only preferred embodiments of the present invention, and the scope of protection of the present invention cannot be limited thereby. Any non-substantial changes and substitutions made by those skilled in the art based on the present invention fall within the scope of protection required by the present invention.

Claims

1. A method for preparing a multifunctional effervescent tablet, characterized in that: The following steps are involved: The effervescent precursor, magnetic material, adsorbent and derivatization agent are mixed evenly and then tableted to obtain the multifunctional effervescent tablet.

2. The method for preparing the multifunctional effervescent tablet according to claim 1, characterized in that: The effervescent precursor is composed of H + donor and CO2 donor; the H + The donor is selected from one or more of sodium dihydrogen phosphate, citric acid, tartaric acid, ascorbic acid, ammonium bicarbonate, and sodium bisulfate; the CO2 donor is selected from one or more of sodium carbonate, sodium bicarbonate, and calcium carbonate; the H + The molar ratio of the donor to the CO2 donor is (1-3):

1.

3. The method for preparing the multifunctional effervescent tablet according to claim 1, characterized in that: The magnetic material is one or more of Fe3O4 nanoparticles, Fe2O3 nanoparticles, CoFe2O4 cobalt ferrite, NiFe2O4 nickel ferrite, and Fe3O4@SiO2 magnetic silicon dioxide.

4. The method for preparing the multifunctional effervescent tablet according to claim 1, characterized in that: The adsorbent is one or more of hydroxylated multi-walled carbon nanotubes, graphene, polypyrrole, polyaniline, metal organic framework materials, and covalent organic framework materials.

5. The method for preparing the multifunctional effervescent tablet according to claim 1, characterized in that: The derivatization reagent is selected from one of fluorescamine, 2,4-dinitrophenylhydrazine and dansyl chloride.

6. The method for preparing the multifunctional effervescent tablet according to any one of claims 1 to 5, characterized in that: The mass ratio of the magnetic material, the adsorbent and the derivatization reagent is (3-5):1:(0.5-2).

7. The method for preparing the multifunctional effervescent tablet according to any one of claims 1 to 5, characterized in that: The uniform mixing is grinding and mixing; the multifunctional effervescent tablet has a diameter of 5 to 20 mm and a thickness of 1 to 10 mm.

8. A multifunctional effervescent tablet prepared by the preparation method according to any one of claims 1 to 7.

9. A use of the multifunctional effervescent tablet as claimed in claim 8, characterized in that: Application in detecting target analytes; the target analytes are aldehyde compounds, ketone compounds or amine compounds.

10. A method for detecting a target analyte using the multifunctional effervescent tablet according to claim 8, characterized in that: The following steps are involved: The sample solution containing the target analyte is treated by adjusting the acidity, and then the multifunctional effervescent tablet is added to perform extraction and derivatization while achieving the effervescent reaction. The derivative product obtained after the treatment is further cleaned and desorbed under the action of an external magnetic field, and the desorbed liquid is then subjected to instrumental analysis, thereby achieving the detection of the target analyte; wherein the effervescent reaction time is 2 to 10 minutes.