Ofloxacin concentration detection method and device, electronic equipment and storage medium

Abstract

The invention relates to the technical field of molecular imaging, in particular to an ofloxacin concentration detection method and device, electronic equipment and a storage medium. The method comprises the following steps: dropwise adding a preset matrix solution to the surface of a to-be-detected sample containing ofloxacin, and carrying out drying treatment in a preset drying mode to obtain a treated to-be-detected sample; performing ionization mass spectrometry imaging analysis on the processed to-be-detected sample in a preset ionization mode by using a preset imaging mass spectrometry microscope to obtain a current signal value; and determining the ofloxacin concentration in the sample to be detected based on a preset ofloxacin concentration-imaging signal value working curve and the current signal value. Therefore, through the good linear relation between the ofloxacin concentration and the signal value of the imaging heat map, the concentration of ofloxacin on the goethite surface can be detected, the problems that an existing detection technology is complex, time-consuming, large in chemical reagent consumption and the like are solved, and the method has the advantages of being high in sensitivity, small in sample use amount, short in analysis response time and the like.

Description

Technical Field

[0001] This application relates to the field of molecular imaging technology, and in particular to a method, apparatus, electronic device and storage medium for detecting ofloxacin concentration. Background Technology

[0002] Quinolone antibiotics are synthetic antibiotics containing a 4-quinolone structure, suitable for both humans and animals. They are also known as pyridoxine or pyridoxine antibiotics. After use in humans or animals, quinolone antibiotics are mostly excreted in their parent form or as metabolic waste, causing harm to the aquatic environment. They can be discharged with sewage, or through surface runoff or wastewater treatment plant effluent, ultimately entering the aquatic environment. Ofloxacin (OFX), an organic compound, is a typical fluoroquinolone antibiotic. These substances are often used in the medical and aquaculture industries due to their strong broad-spectrum antibacterial activity. Although ofloxacin is used for disease prevention and treatment, residual ofloxacin in the aquatic environment also poses potential threats to aquatic plants, animals, and even humans, such as toxicity risks, the development of resistance genes, and allergic reactions.

[0003] Among related technologies, chromatography is the most commonly used method for detecting ofloxacin concentration in environmental samples. It utilizes the different molecular weights, polarities, and flow characteristics of compounds, and employs instruments such as High Performance Liquid Chromatography (HPLC), Ultra High Performance Liquid Chromatography (UHPLC), and Liquid Chromatograph-Mass Spectrometer (LCMS) to separate compounds into different components and perform characteristic analysis using a physical or chemical method, thereby achieving the identification and quantification of chemical substances.

[0004] However, this method cannot directly measure solid samples. It can only convert the sample into a completely dissolved liquid and then extract the target substance through desorption, dissolution and other methods. The processing method is complicated, time-consuming and consumes a lot of chemical reagents, which urgently needs to be solved. Summary of the Invention

[0005] This application provides a method, apparatus, electronic device, and storage medium for detecting ofloxacin concentration, which solves the problems of complex and time-consuming existing detection technologies and high consumption of chemical reagents. It features high sensitivity, small sample volume, and short analysis response time.

[0006] To achieve the above objectives, the first aspect of this application provides a method for detecting ofloxacin concentration, comprising the following steps:

[0007] Obtain the test sample containing ofloxacin;

[0008] A preset matrix solution is dropped onto the surface of the sample to be tested, and the sample is dried using a preset drying method to obtain the processed sample to be tested.

[0009] Using a preset imaging mass spectrometry microscope, the processed sample to be tested is subjected to ionization mass spectrometry imaging analysis in a preset ionization mode to obtain the current signal value;

[0010] The concentration of ofloxacin in the sample to be tested is determined based on the preset ofloxacin concentration-imaging signal value working curve and the current signal value.

[0011] According to one embodiment of this application, before determining the ofloxacin concentration in the sample to be tested based on the preset ofloxacin concentration-imaging signal value working curve and the current signal value, the method further includes:

[0012] A solution of ofloxacin at a preset concentration was dropped onto the surface of goethite in the initial conductive glass slide sample, and then dried using the preset drying method to obtain the first conductive glass slide sample.

[0013] A preset matrix solution is dropped onto the surface of the goethite in the first conductive glass slide sample, and then dried using the preset drying method to obtain the second conductive glass slide sample.

[0014] Using the preset imaging mass spectrometry microscope, the second conductive glass slide sample is subjected to ionization mass spectrometry imaging analysis in the preset ionization mode to obtain the signal value at the mass-to-charge ratio corresponding to the preset concentration of ofloxacin solution.

[0015] Based on the signal values ​​at the mass-to-charge ratio corresponding to ofloxacin solutions under different concentration conditions, the preset ofloxacin concentration-imaging signal value working curve is determined.

[0016] According to one embodiment of this application, before adding the ofloxacin solution of the preset concentration to the goethite surface of the initial conductive glass slide sample, the method further includes:

[0017] Obtain a target glass slide with conductive properties;

[0018] A conductive double-sided adhesive that meets the preset size is attached to the surface of the target glass slide;

[0019] A preset dose of goethite powder is spread evenly on the conductive double-sided adhesive on the surface of the target glass slide and pressed to fix it, thus obtaining an initial conductive glass slide sample with goethite adhering to the surface.

[0020] According to one embodiment of this application, the ratio of the amount of ofloxacin solution added to the preset dose of goethite powder in each sample is 1 mL / g.

[0021] According to one embodiment of this application, the target glass slide is an indium tin oxide glass slide.

[0022] According to the ofloxacin concentration detection method proposed in this application, a preset matrix solution is added to the surface of a sample containing ofloxacin, and then dried using a preset drying method to obtain a processed sample. Next, an ionization mass spectrometry imaging analysis is performed on the processed sample using a preset imaging mass spectrometry microscope in a preset ionization mode to obtain the current signal value. Finally, based on a preset ofloxacin concentration-imaging signal value working curve and the current signal value, the ofloxacin concentration in the sample is determined. Therefore, by utilizing the good linear relationship between the ofloxacin concentration and the signal value of the imaging thermogram, the concentration detection of ofloxacin on the surface of goethite can be achieved, solving the problems of complexity, time consumption, and high chemical reagent consumption in existing detection technologies. This method features high sensitivity, small sample volume, and short analytical response time.

[0023] To achieve the above objectives, a second aspect of this application provides an ofloxacin concentration detection device, comprising:

[0024] The acquisition module is used to acquire test samples containing ofloxacin;

[0025] The processing module is used to drop a preset matrix solution onto the surface of the sample to be tested and to dry it using a preset drying method to obtain the processed sample to be tested.

[0026] The analysis module is used to perform ionization mass spectrometry imaging analysis on the processed sample under a preset ionization mode using a preset imaging mass spectrometry microscope to obtain the current signal value.

[0027] The determination module is used to determine the concentration of ofloxacin in the sample to be tested based on a preset ofloxacin concentration-imaging signal value working curve and the current signal value.

[0028] According to one embodiment of this application, before determining the ofloxacin concentration in the sample to be tested based on the preset ofloxacin concentration-imaging signal value working curve and the current signal value, the determining module further includes:

[0029] The first processing unit is used to drop a solution of ofloxacin of a preset concentration onto the surface of goethite in the initial conductive glass slide sample, and to dry it using the preset drying method to obtain the first conductive glass slide sample.

[0030] The second processing unit is used to drop a preset matrix solution onto the surface of the goethite of the first conductive glass slide sample and perform drying treatment using the preset drying method to obtain the second conductive glass slide sample.

[0031] The analysis unit is used to perform ionization mass spectrometry imaging analysis on the second conductive glass slide sample in the preset ionization mode using the preset imaging mass spectrometry microscope to obtain the signal value at the mass-to-charge ratio corresponding to the preset concentration of ofloxacin solution.

[0032] The determination unit is used to determine the preset ofloxacin concentration-imaging signal value working curve based on the signal value at the mass-to-charge ratio corresponding to ofloxacin solutions under different concentration conditions.

[0033] According to one embodiment of this application, before the ofloxacin solution of the preset concentration is dropped onto the goethite surface of the initial conductive glass slide sample, the first processing unit is further configured to:

[0034] Obtain a target glass slide with conductive properties;

[0035] A conductive double-sided adhesive that meets the preset size is attached to the surface of the target glass slide;

[0036] A preset dose of goethite powder is spread evenly on the conductive double-sided adhesive on the surface of the target glass slide and pressed to fix it, thus obtaining an initial conductive glass slide sample with goethite adhering to the surface.

[0037] According to one embodiment of this application, the ratio of the amount of ofloxacin solution added to the preset dose of goethite powder in each sample is 1 mL / g.

[0038] According to one embodiment of this application, the target glass slide is an indium tin oxide glass slide.

[0039] According to the ofloxacin concentration detection device proposed in this application, a preset matrix solution is dropped onto the surface of a sample containing ofloxacin, and then dried using a preset drying method to obtain a processed sample. Next, an ionization mass spectrometry imaging analysis is performed on the processed sample using a preset imaging mass spectrometry microscope in a preset ionization mode to obtain the current signal value. Finally, based on a preset ofloxacin concentration-imaging signal value working curve and the current signal value, the ofloxacin concentration in the sample is determined. Therefore, by utilizing the good linear relationship between the ofloxacin concentration and the signal value of the imaging thermogram, the concentration detection of ofloxacin on the surface of goethite can be achieved, solving the problems of complexity, time consumption, and high chemical reagent consumption in existing detection technologies. This device features high sensitivity, small sample volume, and short analytical response time.

[0040] To achieve the above objectives, a third aspect of this application provides an electronic device, including: a memory, a processor, and a computer program stored in the memory and executable on the processor, wherein the processor executes the program to implement the ofloxacin concentration detection method as described in the above embodiments.

[0041] To achieve the above objectives, a fourth aspect of this application provides a computer-readable storage medium having a computer program stored thereon, which is executed by a processor to implement the ofloxacin concentration detection method as described in the above embodiments.

[0042] To achieve the above objectives, a fifth aspect of this application provides a computer program product comprising a computer program that, when executed by a processor, is used to implement the ofloxacin concentration detection method as described above.

[0043] Additional aspects and advantages of this application will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of this application. Attached Figure Description

[0044] The above and / or additional aspects and advantages of this application will become apparent and readily understood from the following description of the embodiments taken in conjunction with the accompanying drawings, wherein:

[0045] Figure 1 This is a flowchart of an ofloxacin concentration detection method provided according to an embodiment of this application;

[0046] Figure 2 This is a flowchart of an ofloxacin concentration detection method according to another embodiment of this application;

[0047] Figure 3 This is a schematic diagram of the background mass spectrum of different matrices coated in the presence of a goethite medium, according to an embodiment of this application.

[0048] Figure 4 This is a schematic diagram of an imaging mass spectrum of ofloxacin on a goethite surface when an α-cyano-4-hydroxycinnamic acid matrix solution is coated by dry-drop method according to an embodiment of this application.

[0049] Figure 5 This is a schematic diagram of an imaging thermal image of a goethite surface after gradient dilution of an ofloxacin standard solution according to an embodiment of this application. The coating matrix is ​​α-cyano-4-hydroxycinnamic acid, and the coating method is sublimation.

[0050] Figure 6This is a schematic diagram of an imaging thermal image of ofloxacin on the surface of goethite after adding sodium chloride and potassium chloride solutions according to an embodiment of this application. The coating matrix is ​​α-cyano-4-hydroxycinnamic acid, and the coating method is dry drop method.

[0051] Figure 7 This is a block diagram of the ofloxacin concentration detection device provided according to an embodiment of this application;

[0052] Figure 8 This is a schematic diagram of the structure of an electronic device provided according to an embodiment of this application. Detailed Implementation

[0053] The embodiments of this application are described in detail below. Examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and intended to explain this application, and should not be construed as limiting this application.

[0054] The following description, with reference to the accompanying drawings, describes the ofloxacin concentration detection method, apparatus, electronic device, and storage medium according to embodiments of this application.

[0055] Figure 1 This is a flowchart of an embodiment of the ofloxacin concentration detection method of this application.

[0056] like Figure 1 As shown, the method for detecting ofloxacin concentration includes the following steps:

[0057] In step S101, a test sample containing ofloxacin is obtained.

[0058] First, it is necessary to obtain test samples containing ofloxacin. These samples can be various biological or environmental samples, such as blood, soil, or water samples. These test samples should be prepared for subsequent testing and analysis.

[0059] In step S102, a preset matrix solution is dropped onto the surface of the sample to be tested, and the sample is dried using a preset drying method to obtain the processed sample to be tested.

[0060] Specifically, during sample preparation, a certain amount of a pre-set matrix solution can be added to the sample surface. This matrix solution typically contains specific chemical components that can interact with ofloxacin, thereby enhancing its signal in mass spectrometry analysis. After adding the matrix solution, the sample can be dried using a pre-set drying method to ensure that the matrix solution on the sample surface is uniformly distributed and completely dry, thus obtaining the processed sample, ready for the next step of detection and analysis.

[0061] In step S103, the processed sample to be tested is subjected to ionization mass spectrometry imaging analysis using a preset imaging mass spectrometry microscope in a preset ionization mode to obtain the current signal value.

[0062] Next, the processed sample can be placed under a pre-set imaging mass spectrometry microscope for analysis. This microscope combines mass spectrometry technology to perform high-resolution imaging analysis of the sample surface. During the analysis, an appropriate ionization mode (such as positive ion mode) can be selected to ensure that ofloxacin can be effectively ionized and generate a signal. The signal value of the current sample can then be obtained through analysis using the imaging mass spectrometry microscope.

[0063] In step S104, the concentration of ofloxacin in the sample to be tested is determined based on the preset ofloxacin concentration-imaging signal value working curve and the current signal value.

[0064] Understandably, the signal value obtained in step S103 can indirectly reflect the content of ofloxacin in the sample. To obtain an accurate ofloxacin concentration value, a preset ofloxacin concentration-imaging signal value working curve can be used. This curve, obtained through experimental calibration, can convert the signal value into a specific ofloxacin concentration value. Finally, based on this working curve and the measured current signal value, the ofloxacin concentration in the sample can be determined by interpolation or other mathematical methods. Thus, an accurate ofloxacin concentration value can be obtained, providing important data support for subsequent scientific research or clinical diagnosis.

[0065] To facilitate understanding, the following section provides a detailed explanation of how to obtain the preset ofloxacin concentration-imaging signal value working curve.

[0066] As one possible implementation, in some embodiments, before determining the ofloxacin concentration in the sample to be tested based on a preset ofloxacin concentration-imaging signal value working curve and the current signal value, the method further includes: adding an ofloxacin solution of a preset concentration to the goethite surface of an initial conductive slide sample and drying it using a preset drying method to obtain a first conductive slide sample; adding a preset matrix solution to the goethite surface of the first conductive slide sample and drying it using a preset drying method to obtain a second conductive slide sample; performing ionization mass spectrometry imaging analysis on the second conductive slide sample using a preset imaging mass spectrometry microscope in a preset ionization mode to obtain the signal value at the mass-to-charge ratio corresponding to the preset ofloxacin solution; and determining a preset ofloxacin concentration-imaging signal value working curve based on the signal values ​​at the mass-to-charge ratio corresponding to the ofloxacin solution under different concentration conditions.

[0067] Goethite is a common iron oxide and an important component of environmental minerals. This type of substance is widely distributed in nature, characterized by fine particles, a large specific surface area, and numerous active sites. The coordinating hydroxyl groups on its surface exhibit excellent adsorption properties for antibiotics. This application uses goethite as a medium for in-situ identification of organic matter, aiming to explore its surface adsorption properties and mechanism of action. Furthermore, this method also serves as an in-situ mass spectrometry identification technique to facilitate the detection of organic matter.

[0068] Mass spectrometry (MS) utilizes ionization techniques to convert compounds into charged ions, which are then arranged in order of their proton-to-mass-charge ratio (m / z) to form a spectrum. MS offers advantages such as high sensitivity, small sample volume, short analysis response time, and fast analysis speed for composition and structure analysis. This application utilizes a pre-designed imaging mass spectrometry microscope (such as iMScope TRIO) and matrix-assisted laser desorption / ionization-mass spectrometric imaging (MALDI-MSI) as the MS technique. The basic principle of this technique is to use a specific matrix material to promote the desorption and ionization of the target sample under the influence of an ion source. During this process, molecules in the sample interact with matrix molecules, absorbing laser energy, thereby causing the sample molecules to desorb from the matrix and further ionize into charged particles. These charged particles gain kinetic energy under the influence of an accelerating electric field, forming an ion beam that then enters the mass analyzer. In a mass analyzer, precisely controlled electric and magnetic fields cause charged particles with different mass-to-charge ratios to exhibit opposite velocity dispersion. This dispersion effect causes charged particles with different masses to propagate along different paths in space, ultimately focusing at different locations. By detecting the signal intensity at these focal points, detailed information about the molecular distribution at specific locations on the sample surface can be obtained, ultimately generating a mass spectrum. This mass spectrum allows for the determination of the mass-to-charge ratio of each molecule in the sample, thus enabling rapid and accurate imaging of the molecular distribution at specific locations on the sample surface.

[0069] Specifically, firstly, an initial conductive glass slide sample with goethite uniformly adhered to its surface is prepared. Then, a series of ofloxacin solutions of predetermined concentrations are prepared. These solutions will be used in subsequent experimental steps to ensure accurate detection of the distribution of ofloxacin on the sample surface. After preparing the ofloxacin solutions, a certain volume of ofloxacin solution is dropped onto the goethite surface of the initial conductive glass slide sample. The sample is then dried using a predetermined drying method to obtain the first conductive glass slide sample, which is used for the next experiment. Next, a predetermined matrix solution (such as α-cyano-4-hydroxycinnamic acid (CHCA), 2,5-dihydroxybenzoic acid (DHB), 2,4,6-trihydroxyacetophenone (THAP), etc., are dropped onto the goethite surface of the first conductive glass slide sample, and the sample is then dried as well. A second conductive glass slide sample was obtained. Finally, using a preset imaging mass spectrometry microscope in a preset ionization mode (positive ion mode), ionization mass spectrometry imaging analysis was performed on the second conductive glass slide sample. This yielded the signal values ​​at the mass-to-charge ratio corresponding to the preset concentration of ofloxacin solution. Analysis of these signal values ​​showed a good linear relationship between the signal values ​​of the sample's imaging thermogram and the concentration of ofloxacin solution. Based on the signal values ​​at the mass-to-charge ratio corresponding to ofloxacin solution under different concentration conditions, a preset ofloxacin concentration-imaging signal value working curve could be plotted. Based on this curve, after adding a matrix solution and performing ionization mass spectrometry imaging on goethite or environmental samples containing goethite with unknown ofloxacin concentrations, the concentration of ofloxacin in the sample can be quickly and accurately inferred from the imaging signal values.

[0070] The preset drying method can be air drying, shade drying, or low-temperature drying, but high-temperature drying is not recommended to avoid denaturation or degradation of ofloxacin during sample preparation. During mass spectrometry analysis, the mass-to-charge ratio (MTR) of a specific compound is determined, i.e., the ratio of its mass to its charge. For ofloxacin, the MTR of the measured signal value is the relative molar mass of ofloxacin carrying one unit of positive charge in positive ion detection mode; that is, the MTR of the adduct formed by ofloxacin and one positively charged (cation). The type of cation can be selected according to different research backgrounds and actual environments. Common cations include hydrogen ions (H+), sodium ions (Na+), and potassium ions (K+). These cations are relatively common in real-world environments and are therefore frequently considered in mass spectrometry analysis. By determining the MTR of ofloxacin in the presence of different cations, the concentration of ofloxacin in the sample can be more accurately identified and quantified.

[0071] To prepare an ofloxacin solution of the predetermined concentration, first accurately weigh a certain amount of ofloxacin powder, then dissolve this powder in a selected aqueous solvent. Suitable solvents include purified water (H₂O), a 1:1 volume ratio of acetonitrile (ACN) and water (ACN / H₂O, 1:1, V / V), or a diluted sodium hydroxide solution (dilute NaOH solution). To accelerate dissolution, the solution can be ultrasonically treated in an ultrasonic cleaner for approximately 10 minutes. This method ensures complete dissolution of the ofloxacin powder, resulting in a homogeneous solution with accurate concentration.

[0072] Optionally, in some embodiments, the ratio of the amount of ofloxacin solution added to the preset dose of goethite powder in each sample is 1 mL / g.

[0073] In other words, when adding a pre-concentrated ofloxacin solution to the surface of goethite on the initial conductive glass slide sample, the amount of ofloxacin solution added should be 20 μL. This ensures that the ratio of ofloxacin to goethite is maintained at 1 gram of goethite per milliliter of solution, i.e., the ratio of the amount of ofloxacin solution added to the pre-concentrated dose of goethite powder in each sample is 1 mL / g. This ratio is set to ensure that ofloxacin and goethite react fully in the experiment, thereby achieving the expected experimental results.

[0074] There are several methods for adding the matrix solution during the experiment, including but not limited to the dry drop method, spray gun method, and sublimation method. The choice of these methods depends on the type of matrix used, and no specific limitations are made here. For each sample point, the amount of matrix solution added should be 20 μL, so that the ratio of matrix solution to goethite is maintained at 1 gram of goethite per milliliter of solution, which helps to ensure the accuracy and reliability of the experimental data.

[0075] During the experiment, with ofloxacin solution dropped onto the surface of goethite and coated with an α-cyano-4-hydroxycinnamic acid matrix, the preset ofloxacin concentration-imaging signal value working curve was established at an ofloxacin concentration of 2000 μmol / m. 2 -20μmol / m 2 The concentration exhibits good linearity across the range; therefore, the detection limit for ofloxacin concentration in this application embodiment is determined to be 20 μmol / m³. 2 .

[0076] The following details how to prepare the initial conductive glass slide sample.

[0077] As one possible implementation, in some embodiments, before adding the ofloxacin solution of a preset concentration to the goethite surface of the initial conductive glass slide sample, the method further includes: obtaining a target glass slide with conductive properties; attaching conductive double-sided adhesive that meets a preset size to the surface of the target glass slide; spreading a preset dose of goethite powder on the conductive double-sided adhesive on the surface of the target glass slide and pressing it to fix it, thereby obtaining an initial conductive glass slide sample with goethite adhering to its surface.

[0078] Specifically, firstly, a multimeter (an instrument capable of measuring various electrical parameters) is used to test the conductive surface of the glass slide (a thin glass slide used for microscopic observation) to ensure that the selected target slide possesses the required conductivity. Next, a piece of conductive double-sided tape of a fixed size (e.g., 5mm x 5mm) is selected and adhered to the conductive surface of the target slide. A certain amount (i.e., a pre-set dosage, calibrated) of goethite powder is weighed and evenly spread on the conductive double-sided tape. This process is repeated to create sample spots of uniform size and thickness. Finally, to further ensure a tight bond between the goethite powder and the double-sided tape, the flat end of a double-ended spatula (usually with two differently shaped heads for picking up, placing, and mixing powdered substances) is used to gently press the powder to fix it, thus obtaining the initial conductive glass slide sample.

[0079] It should be noted that, in order to avoid the sample thickness being too thick and affecting the detection sensitivity, the amount of goethite used for each sample point should be 2 mg, and the thickness after uniform spreading should not exceed 15 μm.

[0080] Optionally, in some embodiments, the target glass slide is an indium tin oxide glass slide.

[0081] It is understood that this application selects an indium tin oxide (ITO glass, preferably 25mm*75mm*2mm) glass slide as the target slide. This slide has excellent electrical conductivity and transparency. In addition, it also has good chemical stability and high-temperature resistance, allowing it to remain stable in high-temperature and chemical reaction environments. Therefore, choosing an indium tin oxide glass slide as the experimental substrate material ensures the reliability and validity of the experimental results.

[0082] To facilitate a better understanding of the ofloxacin concentration detection method proposed in the embodiments of this application by those skilled in the art, a detailed description is provided below with reference to specific embodiments.

[0083] like Figure 2As shown, a conductive glass slide sample with iron ore powder adhering to it was first prepared for subsequent imaging detection. Next, an ofloxacin solution of known concentration was prepared and dropped onto the goethite surface of the conductive glass slide sample. After the sample surface was dried, a matrix solution was added (using methods such as dry dropping, spray gun, or sublimation). After the matrix solution coating was completed, the sample was dried. Finally, the treated sample was analyzed by ionization mass spectrometry using an imaging mass spectrometry microscope to obtain the ofloxacin concentration-imaging signal value working curve.

[0084] Based on the above-mentioned basic procedure for ofloxacin concentration detection, the following experiments were conducted in this application.

[0085] Example 1:

[0086] The conductive surface of the indium tin oxide glass slide was measured using a multimeter, and 5mm*5mm conductive double-sided tape was attached to its surface. Then, 2mg of goethite powder was spread evenly on the conductive double-sided tape and gently pressed and fixed with a flat-headed spatula. This process produced a conductive glass slide sample with goethite powder attached, which was then used for subsequent imaging detection.

[0087] Preparation of α-cyano-4-hydroxycinnamic acid matrix solution: The α-cyano-4-hydroxycinnamic acid drug powder can be fully dissolved in a solution of acetonitrile and water mixed in a volume ratio of 1:1 (ACN / H2O, 1:1, V / V) to prepare a 10 g / L matrix solution, and the matrix solution can be stored in a refrigerator at 0℃-4℃ for later use.

[0088] The matrix solution was added using the dry drop method: 20 μL of α-cyano-4-hydroxycinnamic acid matrix solution was dropped onto the surface of goethite, wherein the concentration of α-cyano-4-hydroxycinnamic acid was 10 g / L. After complete drying, it was used for MALDI-MSI imaging analysis.

[0089] Figure 3 (a) shows the background signal peak of α-cyano-4-hydroxycinnamic acid matrix in the presence of goethite medium. The results clearly show that the background signal interference intensity of α-cyano-4-hydroxycinnamic acid matrix is ​​weak in the presence of goethite medium.

[0090] Example 2:

[0091] The conductive glass slide sample with goethite attached was prepared in advance using the method of Example 1.

[0092] Preparation of 2,5-dihydroxybenzoic acid matrix solution: The 2,5-dihydroxybenzoic acid drug powder can be fully dissolved in a solution of acetonitrile and water mixed in a volume ratio of 1:1 (ACN / H2O, 1:1, V / V) to prepare a 10 g / L matrix solution. The prepared matrix solution should be stored in a refrigerator at 0℃-4℃ for later use.

[0093] The matrix solution was added using the dry drop method: 20 μL of 2,5-dihydroxybenzoic acid matrix solution was dropped onto the surface of goethite, with a concentration of 10 g / L. After complete drying, it was used for MALDI-MSI imaging analysis.

[0094] Figure 3 (b) The background signal peaks of the 2,5-dihydroxybenzoic acid matrix in the presence of goethite medium are shown. The results clearly show that the background signal interference intensity of the 2,5-dihydroxybenzoic acid matrix is ​​strong under the participation of goethite medium.

[0095] Example 3:

[0096] The conductive glass slide sample with goethite attached was prepared in advance using the method of Example 1.

[0097] Preparation of 2,4,6-trihydroxyacetophenone matrix solution: The 2,4,6-trihydroxyacetophenone drug powder can be fully dissolved in a solution of methanol and acetonitrile mixed in a volume ratio of 1:1 (MeOH / ACN, 1:1, V / V) to prepare a 10 g / L matrix solution. The prepared matrix solution should be stored in a refrigerator at 0℃-4℃ for later use.

[0098] The matrix solution was added using the dry-drop method: 20 μL of 2,4,6-trihydroxyacetophenone matrix solution was dropped onto the surface of goethite, with the concentration of 2,4,6-trihydroxyacetophenone being 10 g / L. After complete drying, it was used for MALDI-MSI imaging analysis.

[0099] Figure 3 (c) The background signal peaks of the 2,4,6-trihydroxyacetophenone matrix in the presence of goethite medium are shown. The results clearly show that the background signal interference intensity of the 2,4,6-trihydroxyacetophenone matrix is ​​strong in the presence of goethite medium.

[0100] Example 4:

[0101] The conductive glass slide sample with goethite attached and the α-cyano-4-hydroxycinnamic acid matrix solution were prepared in advance using the method of Example 1.

[0102] Preparation of ofloxacin solution: Dissolve ofloxacin powder in a 1:1 volume ratio of acetonitrile and water (ACN / H₂O, 1:1, V / V) to form a 2 mmol / L solution. Before each use, the solution can be sonicated for 10 min in a liquid crystal ultrasonic cleaner to aid dissolution. After use, store in a refrigerator at 0℃-4℃. During experiments, the 2 mmol / L ofloxacin solution can be added dropwise (20 μL) to the surface of goethite using the dry-drop method.

[0103] The matrix solution was added using the dry drop method: 20 μL of α-cyano-4-hydroxycinnamic acid matrix solution was dropped onto the surface of goethite and allowed to dry completely before being used for MALDI-MSI imaging analysis.

[0104] Figure 4 Imaging mass spectrometry was used to detect the imaged mass spectrum of ofloxacin on the surface of goethite when a cyano-4-hydroxycinnamic acid matrix solution was added. In this experiment, when ofloxacin combined with hydrogen ions, a signal associated with ofloxacin was detected at a mass-to-charge ratio of 362.153, indicating that the adduct formed by ofloxacin and hydrogen ions was successfully detected.

[0105] Example 5:

[0106] The conductive glass slide sample with goethite attached and the α-cyano-4-hydroxycinnamic acid matrix solution were prepared in advance using the method of Example 1.

[0107] Prepare a 10 mmol / L ofloxacin standard solution and perform serial dilutions to 5 mmol / L, 1 mmol / L, 500 μmol / L, 100 μmol / L, and 10 μmol / L ofloxacin solutions, with each drop volume being 5 μL.

[0108] The matrix solution was added using the sublimation method: α-cyano-4-hydroxycinnamic acid matrix solution was uniformly coated onto the surface of goethite containing the target contaminant ofloxacin, with consistent coating thickness controlled. A certain amount of α-cyano-4-hydroxycinnamic acid powder was loaded into the slit cavity of a matrix sublimation instrument (such as iMLayerTM), and then the laser source was adjusted to set the matrix coating thickness to 1.0 μm and the sublimation temperature to 250℃. MALDI-MSI instrument parameters were set as follows: laser spot diameter 100 μm, laser intensity 80.5%.

[0109] Figure 5 This example illustrates the imaging thermograms of ofloxacin standard solution after gradient dilution on a goethite surface. The results show that as the ofloxacin standard solution is continuously diluted, the signal value of the imaging thermogram gradually weakens. The lowest detection limit is within the concentration range of ofloxacin solution diluted to 100 μmol / L. At this point, the distribution concentration of ofloxacin at the sample spot is 20 μmol / m³. 2 Imaging results showed that the signal intensity in the imaging thermogram was significantly distorted when ofloxacin solution was added at a concentration of 10 μmol / L. Therefore, the lowest detection limit for MALDI-MSI imaging when ofloxacin solution is added to the surface of goethite and coated with α-cyano-4-hydroxycinnamic acid matrix solution is 20 μmol / L. 2 .

[0110] Example 6:

[0111] Three sets of conductive glass slides with goethite adhering to them were prepared in advance using the method in Example 4. 20 μL of 2 mmol / L ofloxacin solution was added and the samples were allowed to dry completely.

[0112] Prepare 2 mmol / L sodium chloride (NaCl) solution and potassium chloride (KCl) solution respectively. Add an additional 20 μL of sodium chloride solution or potassium chloride solution to each of the two groups of samples. After thorough drying, add 20 μL of 10 g / L α-cyano-4-hydroxycinnamic acid matrix solution to each of the three groups of samples using the dry drop method. After complete drying, perform MALDI-MSI analysis in positive ion mode.

[0113] Figure 6 In this embodiment, three groups of samples were analyzed on the surface of goethite with different mass-to-charge ratios: samples with ofloxacin solution, samples with ofloxacin and potassium chloride solution, and samples with ofloxacin and sodium chloride solution. The results showed that the addition of sodium chloride and potassium chloride solution weakened the thermal imaging signal of the adduct "ofloxacin + hydrogen ions," with sodium chloride solution having a more significant weakening effect. In the control group with only ofloxacin, thermal background values ​​consistent with the mass-to-charge ratios of the adducts "ofloxacin + sodium ions" and "ofloxacin + potassium ions" were found. Comparing these background values ​​with the thermal background values, it was observed that the addition of sodium chloride and potassium chloride solutions resulted in stronger thermal signals in the corresponding groups. This indicates that in positive ion mode, the addition of crystalline salt promotes the formation of new adducts from the positive ions generated by the ionization of ofloxacin and the crystalline salt.

[0114] In summary, the ofloxacin concentration detection method proposed in this application has the following advantages and effects:

[0115] (1) The in-situ mass spectrometry analysis technology used in the embodiments of this application has the characteristics of high sensitivity, short analysis response time, fast analysis speed and small sample amount, which is conducive to the laboratory to carry out the analysis and testing of ofloxacin concentration on solid surface.

[0116] (2) Under the influence of multiple coexisting ions, by screening suitable matrices, the embodiments of this application maintain the characteristics of high selectivity, high sensitivity and low detection limit.

[0117] (3) The chemical reagents involved in the embodiments of this application are mostly common reagents, with low cost and small dosage, resulting in minimal secondary pollution.

[0118] According to the ofloxacin concentration detection method proposed in this application, a preset matrix solution is added to the surface of a sample containing ofloxacin, and then dried using a preset drying method to obtain a processed sample. Next, an ionization mass spectrometry imaging analysis is performed on the processed sample using a preset imaging mass spectrometry microscope in a preset ionization mode to obtain the current signal value. Finally, based on a preset ofloxacin concentration-imaging signal value working curve and the current signal value, the ofloxacin concentration in the sample is determined. Therefore, by utilizing the good linear relationship between the ofloxacin concentration and the signal value of the imaging thermogram, the concentration detection of ofloxacin on the surface of goethite can be achieved, solving the problems of complexity, time consumption, and high chemical reagent consumption in existing detection technologies. This method features high sensitivity, small sample volume, and short analytical response time.

[0119] Next, the ofloxacin concentration detection device according to the embodiments of this application is described with reference to the accompanying drawings.

[0120] Figure 7 This is a block diagram of an ofloxacin concentration detection device according to an embodiment of this application.

[0121] like Figure 7 As shown, the ofloxacin concentration detection device 10 includes: an acquisition module 100, a processing module 200, an analysis module 300, and a determination module 400.

[0122] The acquisition module 100 is used to acquire the test sample containing ofloxacin.

[0123] The processing module 200 is used to drop a preset matrix solution onto the surface of the sample to be tested and to dry it using a preset drying method to obtain the processed sample to be tested.

[0124] The analysis module 300 is used to perform ionization mass spectrometry imaging analysis on the processed sample under a preset ionization mode using a preset imaging mass spectrometry microscope to obtain the current signal value.

[0125] The determination module 400 is used to determine the concentration of ofloxacin in the sample to be tested based on a preset ofloxacin concentration-imaging signal value working curve and the current signal value.

[0126] Furthermore, in some embodiments, before determining the ofloxacin concentration in the sample to be tested based on a preset ofloxacin concentration-imaging signal value working curve and the current signal value, the determining module 400 further includes:

[0127] The first processing unit is used to drop a solution of ofloxacin of a preset concentration onto the surface of goethite in the initial conductive glass slide sample and dry it using a preset drying method to obtain the first conductive glass slide sample.

[0128] The second processing unit is used to drop a preset matrix solution onto the surface of the goethite of the first conductive glass slide sample and perform drying treatment using a preset drying method to obtain the second conductive glass slide sample.

[0129] The analysis unit is used to perform ionization mass spectrometry imaging analysis on the second conductive glass slide sample in a preset ionization mode using a preset imaging mass spectrometry microscope to obtain the signal value at the mass-to-charge ratio corresponding to the preset concentration of ofloxacin solution.

[0130] The determination unit is used to determine the preset ofloxacin concentration-imaging signal value working curve based on the signal value at the mass-to-charge ratio corresponding to ofloxacin solutions under different concentration conditions.

[0131] Furthermore, in some embodiments, before adding a pre-concentrated ofloxacin solution to the goethite surface of the initial conductive glass slide sample, the first processing unit is further configured to:

[0132] Obtain a target glass slide with conductive properties;

[0133] Apply conductive double-sided adhesive that meets the preset size to the surface of the target glass slide;

[0134] A preset dose of goethite powder is spread evenly on the conductive double-sided adhesive on the surface of the target glass slide and pressed to fix it, thus obtaining an initial conductive glass slide sample with goethite adhering to the surface.

[0135] Furthermore, in some embodiments, the ratio of the amount of ofloxacin solution added to the preset dose of goethite powder in each sample is 1 mL / g.

[0136] Furthermore, in some embodiments, the target glass slide is an indium tin oxide glass slide.

[0137] It should be noted that the foregoing explanation of the ofloxacin concentration detection method embodiment also applies to the ofloxacin concentration detection device of this embodiment, and will not be repeated here.

[0138] According to the ofloxacin concentration detection device proposed in this application, a preset matrix solution is dropped onto the surface of a sample containing ofloxacin, and then dried using a preset drying method to obtain a processed sample. Next, an ionization mass spectrometry imaging analysis is performed on the processed sample using a preset imaging mass spectrometry microscope in a preset ionization mode to obtain the current signal value. Finally, based on a preset ofloxacin concentration-imaging signal value working curve and the current signal value, the ofloxacin concentration in the sample is determined. Therefore, by utilizing the good linear relationship between the ofloxacin concentration and the signal value of the imaging thermogram, the concentration detection of ofloxacin on the surface of goethite can be achieved, solving the problems of complexity, time consumption, and high chemical reagent consumption in existing detection technologies. This device features high sensitivity, small sample volume, and short analytical response time.

[0139] Figure 8 A schematic diagram of the structure of an electronic device provided in an embodiment of this application. The electronic device may include:

[0140] The memory 801, the processor 802, and the computer program stored on the memory 801 and capable of running on the processor 802.

[0141] When the processor 802 executes the program, it implements the ofloxacin concentration detection method provided in the above embodiments.

[0142] Furthermore, electronic devices also include:

[0143] Communication interface 803 is used for communication between memory 801 and processor 802.

[0144] The memory 801 is used to store computer programs that can run on the processor 802.

[0145] The memory 801 may include high-speed RAM (Random Access Memory) memory, and may also include non-volatile memory, such as at least one disk storage.

[0146] If the memory 801, processor 802, and communication interface 803 are implemented independently, then the communication interface 803, memory 801, and processor 802 can be interconnected via a bus to complete communication between them. The bus can be an ISA (Industry Standard Architecture) bus, a PCI (Peripheral Component Interconnect) bus, or an EISA (Extended Industry Standard Architecture) bus, etc. The bus can be divided into address bus, data bus, control bus, etc. For ease of representation, Figure 8 The bus is represented by a single thick line, but this does not mean that there is only one bus or one type of bus.

[0147] Optionally, in a specific implementation, if the memory 801, processor 802, and communication interface 803 are integrated on a single chip, then the memory 801, processor 802, and communication interface 803 can communicate with each other through an internal interface.

[0148] The processor 802 may be a CPU (Central Processing Unit), an ASIC (Application Specific Integrated Circuit), or one or more integrated circuits configured to implement the embodiments of this application.

[0149] This application also provides a computer-readable storage medium storing a computer program thereon, which, when executed by a processor, implements the ofloxacin concentration detection method described above.

[0150] This application also provides a computer program product, which includes a computer program that, when executed by a processor, implements the ofloxacin concentration detection method described above.

[0151] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this application, "multiple" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0152] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0153] Although embodiments of this application have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting this application. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of this application.

Claims

1. A method for detecting ofloxacin concentration, characterized in that, Includes the following steps: Obtain the test sample containing ofloxacin; A preset matrix solution is dropped onto the surface of the sample to be tested, and the sample is dried using a preset drying method to obtain the processed sample to be tested. Using a preset imaging mass spectrometry microscope, the processed sample to be tested is subjected to ionization mass spectrometry imaging analysis in a preset ionization mode to obtain the current signal value; The concentration of ofloxacin in the sample to be tested is determined based on the preset ofloxacin concentration-imaging signal value working curve and the current signal value.

2. The method according to claim 1, characterized in that, Before determining the ofloxacin concentration in the sample to be tested based on the preset ofloxacin concentration-imaging signal value working curve and the current signal value, the process further includes: A solution of ofloxacin at a preset concentration was dropped onto the surface of goethite in the initial conductive glass slide sample, and then dried using the preset drying method to obtain the first conductive glass slide sample. A preset matrix solution is dropped onto the surface of the goethite in the first conductive glass slide sample, and then dried using the preset drying method to obtain the second conductive glass slide sample. Using the preset imaging mass spectrometry microscope, the second conductive glass slide sample is subjected to ionization mass spectrometry imaging analysis in the preset ionization mode to obtain the signal value at the mass-to-charge ratio corresponding to the preset concentration of ofloxacin solution. Based on the signal values ​​at the mass-to-charge ratio corresponding to ofloxacin solutions under different concentration conditions, the preset ofloxacin concentration-imaging signal value working curve is determined.

3. The method according to claim 2, characterized in that, Before adding the ofloxacin solution of the preset concentration to the goethite surface of the initial conductive glass slide sample, the procedure further includes: Obtain a target glass slide with conductive properties; A conductive double-sided adhesive that meets the preset size is attached to the surface of the target glass slide; A preset dose of goethite powder is spread evenly on the conductive double-sided adhesive on the surface of the target glass slide and pressed to fix it, thus obtaining an initial conductive glass slide sample with goethite adhering to the surface.

4. The method according to claim 3, characterized in that, The ratio of the amount of ofloxacin solution added to the preset dose of goethite powder in each sample is 1 mL / g.

5. The method according to claim 3, characterized in that, The target glass slide is an indium tin oxide glass slide.

6. An ofloxacin concentration detection device, characterized in that, include: The acquisition module is used to acquire test samples containing ofloxacin; The processing module is used to drop a preset matrix solution onto the surface of the sample to be tested and to dry it using a preset drying method to obtain the processed sample to be tested. The analysis module is used to perform ionization mass spectrometry imaging analysis on the processed sample under a preset ionization mode using a preset imaging mass spectrometry microscope to obtain the current signal value. The determination module is used to determine the concentration of ofloxacin in the sample to be tested based on a preset ofloxacin concentration-imaging signal value working curve and the current signal value.

7. The apparatus according to claim 6, characterized in that, Before determining the ofloxacin concentration in the sample to be tested based on the preset ofloxacin concentration-imaging signal value working curve and the current signal value, the determining module further includes: The first processing unit is used to drop a solution of ofloxacin of a preset concentration onto the surface of goethite in the initial conductive glass slide sample, and to dry it using the preset drying method to obtain the first conductive glass slide sample. The second processing unit is used to drop a preset matrix solution onto the surface of the goethite of the first conductive glass slide sample and perform drying treatment using the preset drying method to obtain the second conductive glass slide sample. The analysis unit is used to perform ionization mass spectrometry imaging analysis on the second conductive glass slide sample in the preset ionization mode using the preset imaging mass spectrometry microscope to obtain the signal value at the mass-to-charge ratio corresponding to the preset concentration of ofloxacin solution. The determination unit is used to determine the preset ofloxacin concentration-imaging signal value working curve based on the signal value at the mass-to-charge ratio corresponding to ofloxacin solutions under different concentration conditions.

8. An electronic device, characterized in that, include: A memory, a processor, and a computer program stored in the memory and executable on the processor, the processor executing the program to implement the ofloxacin concentration detection method as described in any one of claims 1-5.

9. A computer-readable storage medium having a computer program stored thereon, characterized in that, The program is executed by the processor to implement the ofloxacin concentration detection method as described in any one of claims 1-5.

10. A computer program product, characterized in that, The method includes a computer program, which, when executed by a processor, is used to implement the ofloxacin concentration detection method according to any one of claims 1-5.

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