Micro-plastic integrated intelligent detection device

By designing an integrated intelligent fluorescence detection device for microplastics, the sample is enriched using gradient hydrophobic nanocolumn arrays and dynamic self-healing conductive layers, combined with high-sensitive fluorescence detection, the efficient and accurate detection of microplastics is achieved, and the problems of real-time monitoring and high-sensitivity detection in the existing technology are solved, and are suitable for environmental and food safety detection.

CN120369951AActive Publication Date: 2025-07-25WUHAN TEXTILE UNIV

Patent Information

Application Number
CN202510344385.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-21
Publication Date
2025-07-25
Estimated Expiration
2045-03-21

AI Technical Summary

Technical Problem

The existing microplastic detection technology is difficult to achieve real-time monitoring and high-sensitivity detection, and the detection equipment relies on large laboratory instruments, making it difficult to meet the needs of real-time monitoring and food safety detection of microplastic pollution in the environment.

Method used

A microplastic integrated intelligent fluorescence detection device is designed, including a sample pretreatment module, an immune response module and a fluorescence detection module. Combined with an automated control module, a gradient hydrophobic nanocolumn array and a dynamic self-healing conductive layer are used for sample enrichment and detection, and a high-sensitivity time-resolved fluorescence detector is equipped to achieve automated operation and efficient detection.

Benefits of technology

It improves the efficiency and accuracy of microplastic detection, can conduct low-concentration microplastic detection in conventional laboratories or on-site, reduces manual operation errors, and is suitable for environmental monitoring and food safety testing.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a micro-plastic integrated intelligent detection device, which comprises: a sample pretreatment module, which comprises a sample mixing module, a filtering separation module, an enrichment concentration module and a surface modification and marking module which are communicated in sequence and is used for mixing, filtering, enriching, modifying and marking a sample in sequence; the immunoreaction module is used for performing immunoreaction on the sample and the anti-polystyrene monoclonal antibody freeze-dried product marked by the quantum dot fluorescent microspheres; the fluorescence detection module is used for carrying out fluorescence detection on the test strip subjected to the immune reaction; the automatic control module is electrically connected with the sample pretreatment module, the immunoreaction module and the fluorescence detection module and is used for controlling the operation of each module. According to the invention, the sample processing module, the reaction module, the detection module and the control module are in close cooperation, the sample enters each module in sequence after simple pretreatment, detection and result output are semi-automatically completed, frequent manual operation of different instruments is not needed, the operation steps and time are reduced, and the operation difficulty is reduced.
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Description

Technical Field

[0001] The present invention belongs to the technical field of fluorescence detection, and particularly relates to an integrated intelligent fluorescence detection device for microplastics. Background Art

[0002] Microplastics are a new type of environmental pollutant that can adsorb heavy metals and persistent organic pollutants and migrate and transform in the environment. Microplastics have a wide variety of types, great harm, heavy pollution, and a wide range. Microplastics are easily ingested by animals and release the toxic and harmful substances they carry, causing damage to the growth, development, reproduction, gene expression, etc. of organisms. Microplastics have hazards such as sub-lethal toxicity and cytotoxicity, seriously threatening human life and health.

[0003] In China, the environment polluted by microplastics is complex, with large geographical differences and many pollution links, covering fields such as the environment, food, and textiles. During the production process of synthetic fibers (such as polyester fibers, nylon, etc.), some plastic particles or fibers smaller than 5 millimeters may be generated. For example, the friction of production equipment and the incomplete polymerization of raw materials may both lead to the generation of microplastics. In addition, during the textile process, such as spinning, weaving, and dyeing, the operation of machines, the wear of components, and the stress during processing may cause microplastic fibers to fall off the surface of textiles. Especially in some high-intensity processing processes or when using poor-quality raw materials, the possibility of generating microplastics will increase. When people wear textiles, due to body movement, friction, etc., the fibers on the surface of textiles will gradually wear and fall off, generating microplastic fibers. For example, in some frequently rubbed parts, such as cuffs, collars, and trouser legs, fiber shedding is more likely to occur. At the same time, during the washing process in a washing machine, the friction between clothes, the impact of water flow, and the action of detergent will cause a large amount of fibers to fall off from the clothes, forming microplastic fibers. It is estimated that in a typical household washing activity, one piece of clothing can release millions of fibers. Moreover, some synthetic fiber materials, such as nylon and polyester, are more likely to generate microplastic fibers during the washing process due to their fiber structure and characteristics. When waste textiles are landfilled, over time, the textiles will gradually degrade and break in the natural environment, generating microplastics. These microplastics may enter the soil, water bodies and other environments through rainwater scouring and other ways, causing pollution. Although incineration can reduce the amount of solid waste of textiles, during the incineration process, some soot and ash containing microplastics may be generated. If these soot and ash are not properly treated, they will also be released into the environment, causing microplastic pollution.

[0004] Currently, the detection methods for microplastics mainly include: visual method, microscopy, electron microscopy, Raman spectroscopy analysis, infrared spectroscopy, thermal analysis, pyrolysis-gas chromatography / mass spectrometry, laser infrared imaging, and optothermal infrared technology. However, some of these detection techniques can only make qualitative judgments, some have low detection sensitivity, and some rely on large laboratory instruments for detection, making it difficult to monitor the pollution distribution and environmental effects of microplastics in the environment in real time.

[0005] Therefore, an integrated intelligent fluorescence detection device for microplastics is urgently needed. Summary of the Invention

[0006] To solve the defects existing in the prior art, the present invention provides an integrated intelligent fluorescence detection device for microplastics.

[0007] To solve the above technical problems, the present invention provides the following technical solutions:

[0008] The present invention provides an integrated intelligent fluorescence detection device for microplastics, including:

[0009] A sample pretreatment module, including a sample mixing module, a filtration and separation module, an enrichment and concentration module, and a surface modification and labeling module that are connected in sequence, for mixing, filtering, enriching, modifying, and labeling the sample in sequence;

[0010] An immune reaction module, including a fluorescence test strip, a freeze-dried product of anti-polystyrene monoclonal antibody labeled with quantum dot fluorescent microspheres, and a temperature control component, for performing an immune reaction between the sample and the freeze-dried product of anti-polystyrene monoclonal antibody labeled with quantum dot fluorescent microspheres;

[0011] A fluorescence detection module, for performing fluorescence detection on the test strip after the immune reaction;

[0012] An automatic control module, electrically connected to the sample pretreatment module, the immune reaction module, and the fluorescence detection module, for controlling the operation of each module.

[0013] Preferably, the sample mixing module includes a mixing chamber, a stirring paddle, and a mixing motor. The stirring paddle is rotatably arranged in the mixing chamber, and the output shaft of the mixing motor is in transmission connection with the stirring paddle.

[0014] Preferably, the filtration and separation module includes a filtration cylinder, a gradient hydrophobic nano-column array, a micro-groove slip capture channel, a dynamic self-healing conductive layer, and a temperature regulation module. The filtration cylinder is a cylindrical structure, and the upper part of the filtration cylinder is connected to the outlet of the mixing chamber;

[0015] The gradient hydrophobic nanopillar array is a first frustum-shaped substrate structure. A number of first nanowires are provided in the first frustum-shaped substrate. The diameter of the first nanowires is set to gradually decrease from top to bottom. A hydrophobic structure is provided on the inner wall of the first nanowires. The gradient hydrophobic nanopillar array is embedded in the filter cartridge;

[0016] The microgroove slip capture channel is a second frustum-shaped substrate structure. A number of second nanowires are provided in the second frustum-shaped substrate. The diameter of the second nanowires is set to gradually decrease from top to bottom. A plurality of microgrooves are provided on the inner wall of the second nanowires and along the circumferential direction thereof. The microgrooves are composed of a number of rising inclined blocks and are spirally arranged along the axial direction of the second nanowires. A thermosensitive hydrogel is coated in the microgroove slip capture channel; The top of the microgroove slip capture channel and the bottom of the gradient hydrophobic nanopillar array are bonded and connected by plasma treatment;

[0017] The dynamic self-healing conductive layer includes a repair layer, a conductive layer, and a light-responsive layer that are sequentially arranged from top to bottom, and is used to repair its own mechanical damage through the repair agent of the repair layer, and to reorganize the broken grid of the conductive layer through the illumination of the light-responsive layer. After the repair layer, the conductive layer, and the light-responsive layer are sequentially stacked, they are formed into an integrated thin film by ultraviolet curing, and then attached to the bottom of the microgroove slip capture channel through flexible silicone;

[0018] The temperature control module includes a temperature control component and a dynamic control component. The temperature control component includes a temperature sensor, a heating and cooling device, and a temperature controller. The temperature sensor is used to monitor the temperature of the heating and cooling device in real time; The temperature controller is used to control the temperature of the heating and cooling device according to the received signal; The input end of the heating and cooling device is electrically connected to the output end of the temperature controller, and is arranged on the microgroove slip capture channel to adjust the temperature of the hydrogel on the microgroove slip capture channel according to the signal of the temperature controller; The output end of the dynamic control component is electrically connected to the input end of the temperature controller, and includes a microgroove controller and a self-healing controller. The microgroove controller is used to control the heating and cooling device to switch between 4°C and 37°C through the temperature controller; The self-healing controller includes a 405nm LED array and a heating element. The 405nm LED array is used for the repair of the light-responsive layer, and the heating element is used for secondary forming at 60°C.

[0019] Preferably, the repair layer is a polyurethane layer containing microcapsules, and the microcapsules are provided with a hexamethylene diisocyanate repair agent. The conductive layer is a graphene / carbon nanotube conductive grid for detecting the triboelectric signal of microplastics; The light-responsive layer is prepared from a dynamic covalent polymer containing anthracene dimers.

[0020] Preferably, the enrichment and concentration module includes a vacuum chamber, a filter membrane placement platform, and a centrifuge. The inlet of the vacuum chamber is connected to the outlet of the filter cartridge. The filter membrane placement platform is rotatably arranged at the lower end inside the vacuum chamber, and the output shaft of the centrifuge is in transmission connection with the filter membrane placement platform.

[0021] Preferably, the surface modification and labeling module includes a reaction vessel, a sample addition needle, and a reagent storage bottle.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] In the anti-fouling enrichment stage of the present invention, when the water sample flows through the surface of the nano-column, organic substances are repelled by the hydrophobic effect, and microplastics sink to the grooves due to the difference in specific gravity; by alternately switching the magnetic field (changing the inclination angle of the nano-column) and temperature (controlling the roughness of the grooves), the dynamic regulation of "repelling interfering substances - selectively capturing target microplastics" is realized, and the enrichment efficiency is 3 times higher than that of traditional filter membranes.

[0024] In the in-situ detection stage of the present invention, when the captured microplastics slide in the grooves, characteristic voltage signals are generated by friction with the conductive layer (for example, PVC generates -2.1V, and PET is +1.7V). Combining with infrared thermal imaging (friction heat generation difference) enables label-free and rapid classification; the laser-induced breakdown spectroscopy (LIBS) probe is integrated at the end of the groove, and only the retained target particles are ignited for detection, reducing energy consumption.

[0025] In the self-repair and maintenance stage of the present invention, dynamic covalent bond recombination is activated by regular light irradiation (405nm LED array) to repair the material aging caused by long-term use; after the barbs on the grooves are worn, it is heated to 60°C to make the hydrogel reform and restore the microscopic morphology. These treatment methods are efficient and can retain microplastics to the greatest extent, providing high-quality samples for subsequent detection. And the self-repairing characteristics enable it to process samples in extreme environments, improving the detection efficiency and accuracy.

[0026] The present invention is equipped with a high-sensitivity time-resolved fluorescence detector and an advanced optical system, which effectively reduces background interference, improves detection sensitivity, can detect low-concentration polystyrene microplastics, meets the requirements for detecting low-concentration pollutants in environmental monitoring, food safety detection, etc., and improves the detection performance.

[0027] The present invention adopts an automatic control module to enable the microprocessor to be connected to each device through a circuit, achieving automatic control of the device, reducing the complexity and errors of manual operation, and improving work efficiency and detection accuracy. In terms of operation convenience, the man-machine interaction interface adopts a touch screen form, facilitating operation by the operator. The operator can easily set various parameters such as stirring speed, filtration time, vacuum degree, centrifugation speed and time, and sample addition volume. For real-time information feedback, the man-machine interaction interface can display the running state of the device in real time, enabling the operator to understand the working conditions of the device at any time and promptly discover potential problems. At the same time, the fault alarm function can quickly remind the operator when the device malfunctions, facilitating timely measures to solve the problem and reducing downtime and the risk of equipment damage. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 is the overall structural schematic diagram of an integrated intelligent fluorescence detection device for microplastics of the present invention;

[0029] Figure 2 is the overall structural schematic diagram of the sample pretreatment module in the present invention;

[0030] Figure 3 is the top view of the gradient hydrophobic nano-column array in the present invention;

[0031] Figure 4 is the cross-sectional view of the first nano-column in the present invention;

[0032] Figure 5 is the structural schematic diagram of the repair layer in the present invention;

[0033] Figure 6 is the structural schematic diagram of the conductive layer in the present invention;

[0034] Figure 7 is the structural schematic diagram of the light-responsive layer in the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0035] The following describes the preferred embodiments of the present invention with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are only for the purpose of illustrating and explaining the present invention, and are not intended to limit the present invention.

[0036] In the description of the present invention, it should be understood that the orientation or positional relationship indicated by terms such as "left" and "right" is based on the orientation or positional relationship shown in the drawings of the specification. It is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the present invention.

[0037] In the description of the present invention, it should be noted that unless otherwise clearly specified and defined, the terms "installation", "connection", and "linkage" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be directly connected or indirectly connected through an intermediate medium. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0038] As Figures 1 to 7 shown, this embodiment provides a microplastic integrated intelligent fluorescence detection device, which includes a sample pretreatment module 1, an immune reaction module 2, a fluorescence detection module 3, and an automatic control module. The automatic control module includes a microprocessor and a human-machine interface, which are electrically connected to the sample pretreatment module, the immune reaction module, and the fluorescence detection module, and are used to control the operation of each module. The microprocessor is an integrated circuit board, which is installed in an independent control box inside the device. The microprocessor is connected to devices such as motors, solenoid valves, and vacuum pumps of each module through wires to realize the automatic control of the device. The human-machine interface is a touch screen, and the operator can set parameters such as stirring speed, filtration time, vacuum degree, centrifugation speed and time, and sample addition volume through the touch screen. The interface displays information such as the operation status of the device and fault alarm in real time.

[0039] In this embodiment, the sample pretreatment module 1 includes a sample mixing module 11, a filtration and separation module 12, an enrichment and concentration module 13, and a surface modification and labeling module 14 that are connected in sequence, and are used to mix, filter, enrich, modify, and label the sample in sequence.

[0040] As Figure 1 shown, the sample mixing module 11 includes a mixing chamber 111, a stirring paddle 112, and a mixing motor 113. The stirring paddle 112 is rotatably arranged in the mixing chamber 111, and the output shaft of the mixing motor 113 is in transmission connection with the stirring paddle 112. By driving the stirring paddle to rotate through the mixing motor, the samples in the mixing chamber are fully and effectively mixed.

[0041] In this embodiment, the filtration and separation module is a single module, which solves the problem of efficiency loss caused by the separation of the filtration, enrichment, and sensing modules in traditional equipment, and all technologies are based on the cross-border innovative application of existing materials, and have the potential for rapid engineering. The filtration and separation module 12 includes a filter cylinder 121, a gradient hydrophobic nanocolumn array 122, a microgroove slip capture channel 123, a dynamic self-healing conductive layer 124, and a temperature control module 125. The filter cylinder 121 is a cylindrical structure, and the upper part of the filter cylinder 121 is connected to the outlet of the mixing chamber 111.

[0042] As Figure 3As shown, the gradient hydrophobic nanopillar array 122 is a first frustum-shaped substrate structure. A number of first nanowires are provided in the first frustum-shaped substrate. The diameter of the first nanowires is set to gradually decrease from top to bottom. A hydrophobic structure is provided on the inner wall of the first nanowires. The gradient hydrophobic nanopillar array 122 is embedded in the filter cartridge 121. The hydrophobic structure is the hydrophobic structure on the surface of a lotus leaf or other existing hydrophobic structures, and no specific limitation is made. Use electron beam lithography or laser etching technology to fabricate a first frustum-shaped nanopillar template (with grooves matching the hydrophobic structure on the surface) on a silicon wafer. Mix a polydimethylsiloxane substrate material and magnetic nanoparticles (such as Fe3O4) in a weight ratio of 10:1, inject it into the template cavity, and demold after high-temperature curing to form a gradient hydrophobic nanopillar array doped with magnetic particles. Coat fluorosilane to reduce the surface energy and enhance the hydrophobicity.

[0043] As Figure 6 As shown, the microgroove slip capture channel 123 is a second frustum-shaped substrate structure. A number of second nanowires are provided in the second frustum-shaped substrate. The diameter of the second nanowires is set to gradually decrease from top to bottom. A plurality of microgrooves are provided on the inner wall of the second nanowires and along the circumferential direction thereof. The microgrooves are composed of a number of rising inclined blocks and are spirally arranged along the axial direction of the second nanowires. A thermosensitive hydrogel is coated on the inner wall of the microgroove slip capture channel 123. The top of the microgroove slip capture channel 123 and the bottom of the gradient hydrophobic nanopillar array 122 are bonded and connected by plasma treatment. Use electron beam lithography or laser etching technology to fabricate a second frustum-shaped nanopillar template (with grooves matching the rising inclined blocks on the surface) on a silicon wafer. Mix a polydimethylsiloxane substrate material and magnetic nanoparticles (such as Fe3O4) in a weight ratio of 10:1, inject it into the template cavity, and demold after high-temperature curing to form a microgroove slip capture channel. Coat fluorosilane to reduce the surface energy and enhance the hydrophobicity.

[0044] The dynamic self-healing conductive layer 124 is used to release a repair agent through a repair layer to repair its own mechanical damage (such as material fracture caused by scratches and cracks), and to recombine the broken grid of the conductive layer through the illumination of a light-responsive layer. As Figures 5 to 7As shown, the dynamic self-healing conductive layer 124 includes a repair layer 1241, a conductive layer 1242, and a light-responsive layer 1243 arranged in sequence from top to bottom. The repair layer 1241, the conductive layer 1242, and the light-responsive layer 1243 are stacked in sequence and then form an integrated film through ultraviolet curing, and then are attached to the bottom of the microgroove slip capture channel 123 through flexible silica gel. Among them, the repair layer 1241 is a polyurethane layer containing microcapsules, and a hexamethylene diisocyanate repair agent is provided inside the microcapsules. The conductive layer 1242 is a graphene / carbon nanotube conductive network for detecting microplastic triboelectric signals. The light-responsive layer 1243 is prepared from a dynamic covalent polymer containing anthracene dimers. Its self-healing property makes it suitable for extreme environments with complex media such as oily sewage and high-salt seawater; and because the composite film is small in size and convenient to carry, the composite film can be made into a wristband sampler to monitor the personal drinking water microplastic exposure in real time.

[0045] In this embodiment, the temperature control module 125 is used to control the temperatures of the filtration and separation module and the light-responsive layer. The temperature control module 125 includes a temperature control component and a dynamic control component. The temperature control component includes a temperature sensor, a heating and cooling device, and a temperature controller. The temperature sensor is used to monitor the temperature of the heating and cooling device in real time. The temperature controller is used to control the temperature of the heating and cooling device according to the received signal. The input end of the heating and cooling device (electric heating sheet and semiconductor cooler) is electrically connected to the output end of the temperature controller, and it is arranged on the microgroove slip capture channel and is used to adjust the temperature of the hydrogel on the microgroove slip capture channel according to the signal of the temperature controller, so as to perform the following temperature control on the hydrogel:

[0046] (1) 4°C low-temperature state: The hydrogel swells, and the inner wall of the groove is smooth, promoting the rapid sliding of microplastics towards the detection area;

[0047] (2) 37°C high-temperature state: The hydrogel shrinks, exposing the barbed structure, and selectively capturing target microplastics (such as PE fibers);

[0048] (3) 60°C repair temperature: Heating causes the hydrogel to be re-shaped and restores the microscopic morphology of the groove.

[0049] The output end of the dynamic control component is electrically connected to the input end of the temperature controller, and includes a microgroove regulator and a self-healing regulator. The microgroove regulator is used to control the heating and cooling device to switch between 4°C and 37°C through the temperature controller, thereby changing the state of the hydrogel. The self-healing regulator includes a 405nm LED array and a heating element. The 405nm LED array is used for the repair of the light-responsive layer, and the heating element is used for the secondary shaping at 60°C. Through photoactivation of the dynamic covalent bond recombination, the damage of the conductive layer is repaired (no direct temperature control, but it needs to cooperate with heating).

[0050] In this embodiment, the enrichment and concentration module 13 includes a vacuum chamber 131, a filter membrane placement platform 132, and a centrifuge 133. The inlet of the vacuum chamber 131 is connected to the outlet of the filter cartridge 121. The filter membrane placement platform 132 is rotatably arranged at the lower end inside the vacuum chamber 131, and the output shaft of the centrifuge 133 is in transmission connection with the filter membrane placement platform 132. The vacuum chamber is a sealed container. The top of the vacuum chamber is connected to a vacuum pipeline, and the internal air is pumped out by a vacuum pump to reduce the pressure. The filter membrane placement platform is used to place the filter membrane for intercepting nanoplastics. There are grooves on the platform surface to ensure that the filter membrane fits tightly and prevent solution leakage. The centrifuge has multiple centrifuge tube slots. The centrifuge tubes are made of high-strength plastic and are adapted to the size of the filter membrane. The rotation speed and time of the centrifuge are set by an automated control module.

[0051] In this embodiment, the surface modification and labeling module 14 includes a reaction vessel, a sampling needle, and reagent storage bottles. The reaction vessel is a glass container, which is connected to the outlet of the enrichment and concentration module. The container is equipped with a sealed lid to prevent solution volatilization. The sampling needle is made of high-precision stainless steel and can accurately aspirate and add modifier and labeling agent solutions. Multiple reagent storage bottles are neatly arranged on one side of the device and store different reagents such as chromogenic agents and labeled antibodies respectively. The storage bottles are connected to the sampling needle through pipelines, and solenoid valves are provided on the pipelines to control the reagent flow rate.

[0052] In this embodiment, the immune reaction module 2 includes a fluorescence test strip, a freeze-dried product of anti-polystyrene monoclonal antibody labeled with quantum dot fluorescent microspheres, and a constant temperature control component, which is used to carry out an immune reaction between the sample and the freeze-dried product of anti-polystyrene monoclonal antibody labeled with quantum dot fluorescent microspheres and maintain a stable reaction environment at 37°C to ensure that the immune reaction proceeds under optimal conditions; the fluorescence detection module 3 is used to perform fluorescence detection on the test strip after the immune reaction. The anti-polystyrene monoclonal antibody in the freeze-dried product of anti-polystyrene monoclonal antibody is secreted by the hybridoma cell line PS-17. The preservation number of the hybridoma cell line PS-17 is CCTCC NO: C2024145, the preservation date is May 10, 2024, the preservation unit is the China Center for Type Culture Collection, and the address of the preservation unit is inside Wuhan University, No. 299, Bayi Road, Wuchang District, Wuhan City, Hubei Province.

[0053] The fluorescence detection module is equipped with existing high-sensitivity time-resolved fluorescence detectors, such as the time-resolved fluorescence microplate reader produced by BMG LABTECH and the high-precision ATP fluorescence detector of Ningbo Boao Bioengineering Co., Ltd. It can quickly and accurately detect the fluorescence intensities of the test line (T) and the quality control line (C) on the fluorescence immunochromatographic test strip. By adopting an advanced optical system, background interference is effectively reduced, and the sensitivity and accuracy of detection are improved. The detection data is transmitted to the data processing module in real time for subsequent analysis.

[0054] The working principle of this embodiment will be further described as follows:

[0055] Instrument assembly: Assemble the sample pretreatment module 1, immune reaction module 2, fluorescence detection module 3, and automatic control module 4 according to the design requirements to ensure tight connections and normal communication between the modules. During the assembly process, strictly debug and calibrate each module to ensure the stable and reliable performance of the instrument.

[0056] Reagent preparation: Prepare freeze-dried products of anti-polystyrene monoclonal antibodies labeled with quantum dot fluorescent microspheres and load them into the sample reaction bottles. Prepare various reagents such as sample diluent, coating buffer, and blocking solution, and store them in the corresponding reagent storage containers respectively to ensure the quality and stability of the reagents.

[0057] Liquid sample detection: Pour the liquid sample into the sample input port of the sample processing module, and the instrument automatically performs centrifugation at 17,000×g for 3 minutes to separate the supernatant. The supernatant is transported to the reaction module through the automatic sampling system and mixed with the freeze-dried products of anti-polystyrene monoclonal antibodies labeled with quantum dot fluorescent microspheres in the sample reaction bottles, and reacts at 37°C for 6 - 10 minutes. After the reaction, insert the fluorescence test strip into the reaction module. After the reaction is completed, send the test strip into the detection instrument for fluorescence intensity detection.

[0058] Solid and semi-solid sample detection: Put the solid or semi-solid sample into the sample processing chamber of the sample processing module, add an appropriate amount of digestion reagent, and process it according to the preset digestion procedure. After digestion, obtain the microplastic sample through steps such as filtration and extraction, and then dilute it to an appropriate concentration with the sample diluent. Transport the diluted sample to the reaction module, and the subsequent operations are the same as those for liquid sample detection.

[0059] Data processing and result output: The fluorescence detection module transmits the detected fluorescence intensity data to the data processing module, displays the T / C value, and obtains the concentration of polystyrene microplastics in the sample according to the built-in standard curve. The user can view the detection results on the display screen of the data processing module or export the data to an external storage device.

[0060] (1) This embodiment compares with the microplastic in-situ characterization technology (such as the mIRage system).

[0061] Process efficiency: The mIRage system relies on non-contact submicron infrared Raman synchronous analysis. Although it does not require complex sample preparation (directly filter and load onto the machine), it only characterizes the enriched samples and lacks a pretreatment automation module. This design covers the entire process from mixing, filtering to detection, and the single-sample processing time < 30 minutes, which is more suitable for batch detection requirements.

[0062] Application scenarios: mIRage is applicable to scientific research-level in-situ chemical analysis (such as the identification of microplastics in brain tissue), while this device focuses more on the rapid screening and quantitative detection of environmental and biological samples.

[0063] (2) This embodiment compares with the carbon nanotube thin film detection device.

[0064] Functional integration: The carbon nanotube thin film detection device of Zhongneng Hydrogen Sink focuses on the convenience of temperature detection (such as the quick disassembly and assembly of hydraulic push rods), but has a single function and is only for material property testing. This device integrates multiple module functions (such as surface modification, immune reaction) and supports the synchronous analysis of the chemical properties and biological toxicity of nanoplastics.

[0065] Intelligent level: The carbon nanotube device has not integrated automated control and data intelligent analysis functions, while this design realizes multi-task scheduling through the ARM Cortex-M7 microprocessor, pre-sets standardized detection protocols, and reduces the operation complexity.

[0066] (3) This embodiment compares with traditional vision detection devices.

[0067] Detection dimension: Machine vision detection devices (such as the appearance defect detection of rubber and plastic parts) rely on optical imaging and are suitable for macroscopic morphology analysis, but cannot detect the chemical composition of nanoscale plastics. This device realizes the molecular-level recognition of nanoplastics through fluorescence immunochromatography technology combined with specific antibody labeling.

[0068] Sensitivity and anti-interference ability: Traditional vision devices are easily affected by light and background noise, while this design adopts time-resolved fluorescence technology, effectively shields short-lived background fluorescence through delayed signal acquisition, and significantly improves the signal-to-noise ratio.

[0069] (4) This embodiment compares with synchrotron nanomaterial testing devices.

[0070] Cost and portability: Synchrotron devices (such as in-situ gas-phase growth testing) rely on large-scale equipment and high-energy radiation sources and require a professional laboratory environment. This device is compact, suitable for conventional laboratories or on-site detection, and has a lower cost.

[0071] Detection object: Synchrotron technology is mainly used for material structure analysis (such as phase change processes), while this design is for the biocompatibility and toxicity assessment of nanoplastics, and the application scenarios are complementary.

[0072] Finally, it should be noted that the above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or perform equivalent replacements for some of the technical features. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. An integrated intelligent detection device for microplastics, characterized in that, Including: A sample pretreatment module (1), including a sample mixing module (11), a filtration and separation module (12), an enrichment and concentration module (13), and a surface modification and labeling module (14) that are connected in sequence, for mixing, filtering, enriching, modifying, and labeling the sample in sequence; An immunoreaction module (2), including a fluorescent test strip, a freeze-dried product of anti-polystyrene monoclonal antibody labeled with quantum dot fluorescent microspheres, and a constant temperature control component, for performing an immunoreaction between the sample and the freeze-dried product of anti-polystyrene monoclonal antibody labeled with quantum dot fluorescent microspheres; A fluorescence detection module (3), for performing fluorescence detection on the test strip after the immunoreaction; An automatic control module, electrically connected to the sample pretreatment module, the immunoreaction module, and the fluorescence detection module, for controlling the operation of each module.

2. The microplastic integrated intelligent detection device according to claim 1, wherein, The sample mixing module (11) includes a mixing chamber (111), a stirring paddle (112), and a mixing motor (113). The stirring paddle (112) is rotatably arranged in the mixing chamber (111), and the output shaft of the mixing motor (113) is in transmission connection with the stirring paddle (112).

3. The integrated intelligent microplastic detection device according to claim 2, characterized in that, The filtration and separation module (12) includes a filter cylinder (121), a gradient hydrophobic nano-column array (122), a micro-groove slip capture channel (123), a dynamic self-healing conductive layer (124), and a temperature control module (125). The filter cylinder (121) is a cylindrical structure, and the upper part of the filter cylinder (121) is connected to the outlet of the mixing chamber (111); The gradient hydrophobic nano-column array (122) is a first frustum-shaped substrate structure. There are several first nano-columns in the first frustum-shaped substrate. The diameter of the first nano-columns is arranged from large to small from top to bottom. The inner wall of the first nano-columns is provided with a hydrophobic structure. The gradient hydrophobic nano-column array (122) is embedded in the filter cylinder (121); The micro-groove slip capture channel (123) is a second frustum-shaped substrate structure. There are several second nano-columns in the second frustum-shaped substrate. The diameter of the second nano-columns is arranged from large to small from top to bottom. A plurality of micro-grooves are provided on the inner wall and the circumferential direction of the second nano-columns. The micro-grooves are composed of several rising inclined blocks and are spirally arranged along the axial direction of the second nano-columns. The micro-groove slip capture channel (123) is coated with a temperature-sensitive hydrogel; the top of the micro-groove slip capture channel (123) is bonded to the bottom of the gradient hydrophobic nano-column array (122) through plasma treatment; The dynamic self-healing conductive layer (124) includes a repair layer (1241), a conductive layer (1242), and a light-responsive layer (1243) arranged in sequence from top to bottom, for releasing a repair agent through the repair layer to repair its own mechanical damage, and recombining the broken grid of the conductive layer through the illumination of the light-responsive layer; The temperature control module (125) includes a temperature control component and a dynamic control component. The temperature control component includes a temperature sensor, a heating and cooling device, and a temperature controller. The temperature sensor is used to monitor the temperature of the heating and cooling device in real time; the temperature controller is used to control the temperature of the heating and cooling device according to the received signal; the input end of the heating and cooling device is electrically connected to the output end of the temperature controller, and it is arranged on the microgroove slip capture channel and is used to adjust the temperature of the hydrogel on the microgroove slip capture channel according to the signal of the temperature controller; the output end of the dynamic control component is electrically connected to the input end of the temperature controller, and includes a microgroove regulator and a self-healing regulator. The microgroove regulator is used to control the heating and cooling device to switch between 4°C and 37°C through the temperature controller; the self-healing regulator includes a 405nm LED array and a heating element. The 405nm LED array is used for the repair of the photo-responsive layer, and the heating element is used for secondary forming at 60°C.

4. The microplastic integrated intelligent detection device according to claim 3, characterized in that, The repair layer (1241) is a polyurethane layer containing microcapsules, and a hexamethylene diisocyanate repair agent is provided inside the microcapsules. The conductive layer (1242) is a graphene / carbon nanotube conductive grid and is used for the detection of microplastic triboelectric signals; the photo-responsive layer (1243) is prepared from a dynamic covalent polymer containing anthracene dimers.

5. An integrated intelligent microplastic detection device according to claim 4, characterized in that, The enrichment and concentration module (13) includes a vacuum chamber (131), a filter membrane placement platform (132), and a centrifuge (133). The inlet of the vacuum chamber (131) is connected to the outlet of the filter cartridge (121). The filter membrane placement platform (132) is rotatably arranged at the lower end inside the vacuum chamber (131), and the output shaft of the centrifuge (133) is in transmission connection with the filter membrane placement platform (132).

6. The microplastic integrated intelligent detection device according to claim 5, characterized in that, The surface modification and labeling module (14) includes a reaction vessel, a sampling needle, and a reagent storage bottle.

Citation Information

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