CN117946516A - Polyurethane fluorescent optical imitation - Google Patents
Polyurethane fluorescent optical imitation Download PDFInfo
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- CN117946516A CN117946516A CN202410349810.1A CN202410349810A CN117946516A CN 117946516 A CN117946516 A CN 117946516A CN 202410349810 A CN202410349810 A CN 202410349810A CN 117946516 A CN117946516 A CN 117946516A
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- Materials For Medical Uses (AREA)
Abstract
The invention discloses a polyurethane fluorescent optical imitation body which is in a multi-grid structure, wherein each unit grid of the multi-grid is provided with a fluorescent imitation body; the concentration of the fluorescent dye in the fluorescent imitation bodies in different unit cells changes in a gradient manner; or, the concentrations of the fluorescent dyes in the different fluorescent sensitivity imitators are the same, the depth of the fluorescent imitators, the diameter of the fluorescent imitators or the depth of the imitators which are not doped with the fluorescent dye and have scattering coefficient and absorption coefficient on the fluorescent sensitivity imitators with the same depth are in gradient change; the preparation process of the fluorescence sensitivity imitation comprises the following steps: heating the polyurethane curing agent and the polyurethane prepolymer in a vacuum state respectively to remove water; uniformly mixing the fluorescent dye, the polyurethane curing agent and the polyurethane prepolymer in a preset proportion, adding the mixture into a cell, and curing after air bubble pumping.
Description
Technical Field
The invention belongs to the field of tissue optical imitation, and particularly relates to a polyurethane fluorescent optical imitation.
Background
The fluorescent imaging has strong specificity and high sensitivity, and is used for diagnosing and treating diseases. In surgical navigation, fluorescence imaging guides the progress of surgery and improves the therapeutic effect of surgery by displaying markers. Indocyanine green (ICG) is a dye approved by the U.S. Food and Drug Administration (FDA) for use in humans, is also a near infrared fluorescent dye, has a deep penetration depth, and can be used for in vivo tumor imaging. The system construction, performance index measurement and performance calibration of the imaging system are considered before clinical use. Fluorescent optical mimics can facilitate investigation of fluorescent imaging systems. IR-125 is similar to ICG in structure, belongs to cyanine dye, has excellent bleaching resistance, and takes the combination capability of fluorescent dye and matrix into consideration, wherein IR-125 is fluorescent dye, polyurethane is selected as matrix, and polyurethane has long-term optical stability and mechanical stability. When the polyurethane is combined with IR-125, the quality similar to bubbles exists in the manufactured imitation body due to the existence of moisture and gas in the material, and the fluorescent imitation body with various functions is also beneficial to improvement and measurement of a fluorescent imaging system, performance comparison among different imaging systems and performance calibration of the imaging system.
Disclosure of Invention
In order to solve the above problems, an object of an embodiment of the present application is to provide a polyurethane fluorescent optical imitation.
The application provides a polyurethane fluorescent optical imitation body which is in a multi-grid structure, wherein each unit grid of the multi-grid is provided with a fluorescent imitation body;
the concentration of the fluorescent dye in the fluorescent imitation bodies in different unit cells changes in a gradient manner; or alternatively, the first and second heat exchangers may be,
The concentrations of the fluorescent dyes in the fluorescent simulants in different unit cells are the same, and the depth of the fluorescent simulants, the diameter of the fluorescent simulants or the depth of the simulants with the same depth, which are not doped with the fluorescent dyes and have scattering coefficients and absorption coefficients, are changed in a gradient manner;
All fluorescent mimics of Gong Gezhong constitute fluorescent sensitivity mimics;
the preparation process of the fluorescent imitation comprises the following steps:
heating the polyurethane curing agent and the polyurethane prepolymer in a vacuum state respectively to remove water;
Uniformly mixing the fluorescent dye, the polyurethane curing agent and the polyurethane prepolymer in a preset proportion, adding the mixture into a cell, and curing after air bubble pumping.
Further, for fluorescent sensitivity mimics in which the concentration of fluorescent dye in the fluorescent mimics in different cells is changed in a gradient, the preparation process comprises:
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution respectively in a vacuum state to remove the water in the polyurethane prepolymer and the polyurethane cross-linking agent;
uniformly mixing fluorescent dyes with different masses with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring into different cells in a multi-grid, wherein the concentration of the fluorescent dye in the fluorescent imitation in each cell is in gradient change, the depth is the same and the diameter is the same, and extracting bubbles for curing.
Further, the fluorescent sensitivity imitators with the same concentration of fluorescent dye and gradient change of depth of the fluorescent imitators in different unit cells are prepared by the following steps:
Adding a scattering medium and an absorption medium into the polyurethane crosslinking agent, and fully and uniformly stirring to obtain a polyurethane crosslinking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution added with the scattering medium and the absorption medium in a vacuum state respectively to remove the moisture in the polyurethane prepolymer and the polyurethane cross-linking agent;
Uniformly mixing fluorescent dye with the same mass with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring the mixture into different cells in a multi-grid, wherein the pouring depth of each cell is in gradient change, the fluorescence concentration is the same, the diameter is the same, and curing is performed after air bubbles are extracted.
Further, for the fluorescent sensitivity imitators which have no fluorescent dye doping on the same-depth fluorescent imitators and have gradient change of depth of imitators with scattering coefficient and absorption coefficient, two layers are divided into each cell, and the lower layers are fluorescent imitators with the same fluorescent dye concentration, the same depth and the same diameter in different cells; the upper layer is a non-fluorescent imitation body which does not contain fluorescent dye, contains scattering property and absorption property and has gradient change of depth in different cells, and the fluorescent imitation bodies in all the cells jointly form a depth sensitivity imitation body, and the preparation process comprises the following steps:
Adding a scattering medium and an absorption medium into the polyurethane crosslinking agent, and fully and uniformly stirring to obtain a polyurethane crosslinking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution added with the scattering medium and the absorption medium in a vacuum state respectively to remove the moisture in the polyurethane prepolymer and the polyurethane cross-linking agent;
uniformly mixing fluorescent dye with the same mass with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring the mixed solution and polyurethane prepolymer into different cells in a multi-grid, pouring the mixed solution and polyurethane prepolymer into each cell with the same depth and diameter, extracting bubbles and curing;
The polyurethane cross-linking agent mixed solution and the polyurethane prepolymer with corresponding proportions are uniformly mixed and respectively poured into different cells in the multi-cell, the pouring depth of each cell is in gradient change and the diameter is the same, and the cells are solidified after being extracted, wherein the scattering coefficient and the absorption coefficient of an imitation body formed by twice solidification in each cell are the same.
Further, the fluorescent imitators in different unit cells have the same fluorescent dye concentration and the fluorescent imitators have gradient diameters, and the preparation process comprises the following steps:
Adding a scattering medium and an absorption medium into the polyurethane crosslinking agent, and fully and uniformly stirring to obtain a polyurethane crosslinking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution added with the scattering medium and the absorption medium in a vacuum state respectively to remove the moisture in the polyurethane prepolymer and the polyurethane cross-linking agent;
uniformly mixing fluorescent dyes with the same mass with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring the mixed solution and polyurethane prepolymer into different cells in a multi-cell grid, extracting bubbles, and solidifying, wherein the diameter of each cell is in gradient change, and the concentration and depth of the fluorescent dyes are the same.
Further, the fluorescent sensitivity imitators with the same scattering coefficient are prepared by the steps of:
Adding scattering media with the same mass into a plurality of polyurethane cross-linking agents, and fully and uniformly stirring to form polyurethane cross-linking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution respectively in a vacuum state to remove the water in the polyurethane prepolymer and the polyurethane cross-linking agent;
Uniformly mixing fluorescent dye with gradient change quality with polyurethane prepolymer and polyurethane cross-linking agent mixed solution in a preset proportion, respectively pouring the mixture into different cells of a multi-cell grid, and extracting bubbles for solidification, wherein the concentration of the dye poured into each cell grid is gradient change, the depth is the same, and the diameter is the same.
Further, the fluorescent sensitivity imitation body with the same scattering coefficient and absorption coefficient, wherein the concentration of the fluorescent dye in the fluorescent imitation body in different unit cells is changed in a gradient manner, and the preparation process comprises the following steps:
respectively adding scattering medium and absorption medium with the same mass into a plurality of polyurethane cross-linking agents, and fully and uniformly stirring to form polyurethane cross-linking agent mixed solution;
respectively heating polyurethane prepolymer and polyurethane cross-linking agent mixed solution with gradient change of absorption medium concentration in vacuum state to remove water in polyurethane prepolymer and polyurethane cross-linking agent;
Uniformly mixing fluorescent dye with gradient mass and polyurethane prepolymer and polyurethane cross-linking agent mixed solution in a preset proportion, respectively pouring the mixed solution into different cells of the multi-cell, and extracting bubbles for curing.
Further: the ratio of the polyurethane prepolymer to the polyurethane crosslinking agent is 1:2-2:1.
Further: heating and dehydrating under vacuum, setting 90-100 ℃ and duration 10 h-36 h;
after vacuum high-temperature dehydration is carried out before the polyurethane prepolymer and the polyurethane crosslinking agent are mixed, the moisture content is controlled below 0.02 percent, and after the polyurethane prepolymer and the polyurethane crosslinking agent are mixed, an air bubble extracting instrument is utilized to extract bubbles in the mixed solution;
curing is retarded by controlling the temperature of the polyurethane prepolymer and the polyurethane crosslinking agent prior to mixing them. The application also provides a fluorescent optical imitation body, which is obtained by spin coating a plurality of layers of films on the surface of the multi-grid of the polyurethane fluorescent optical imitation body, wherein the thickness, the scattering coefficient and the absorption coefficient of each layer are different, and the film material is polyurethane, PDMS, polyester or PMMA.
The technical scheme provided by the embodiment of the application can comprise the following beneficial effects:
As can be seen from the above embodiments, the fluorescent polyurethane manufactured by the present application simulates fluorescent intensities of different fluorescent concentrations or the same concentrations and different depths or different diameters, and the emission wavelength of ICG, so as to further realize the fluorescent concentration sensitivity, the fluorescent depth sensitivity, and the field size of the imaging system, and the scattering material and the absorbing material are added into the imitation body, so that the optical parameters (refractive index, scattering coefficient and absorption coefficient) can be simulated, the fluorescent imaging system can be used for testing the performance parameters, sensitivity, fluorescent intensity and fluorescent wavelength of the fluorescent imaging system, and the manufactured fluorescent imitation body can also be used for performing space three-dimensional imaging on the fluorescent imaging system, and can be used for performing performance calibration on the fluorescent imaging system (two-photon imaging, confocal, wide-field fluorescent imaging, and multiphoton imaging). The polyurethane fluorescent optical imitation body has the advantages that the multi-grid surface is spin-coated with a plurality of films, so that structural imaging can be carried out on an optical coherence tomography imaging system and a photoacoustic imaging system, and the longitudinal resolution and the imaging depth can be measured. The manufacturing method of the fluorescent imitation body has the advantages of high quality, high precision, no bubbles, capability of solving the problem of a large number of bubbles in the polyurethane fluorescent imitation body, capability of manufacturing imitation bodies with any concentration, capability of manufacturing imitation bodies with any shape on plastic grinding tools with any shape, capability of controlling thickness of the imitation bodies, capability of adjusting scattering coefficient and absorption coefficient, high repeatability, high precision, high controllability, capability of mass production, low cost, capability of calibrating fluorescent characteristics under different tissue depths, and capability of measuring and calibrating optical coherence tomography.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the application as claimed.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application.
FIG. 1 is a schematic diagram of a 9-grid polyurethane fluorescent optical imitation with different IR-125 concentrations.
FIG. 2 is a schematic diagram of a 9-grid polyurethane fluorescent optical imitation with different IR-125 concentrations and the same scattering coefficient.
FIG. 3 is a schematic diagram of a 9-grid polyurethane fluorescent optical imitation with different IR-125 concentrations, identical scattering coefficients and absorption coefficients.
FIG. 4 is a schematic diagram of a 9-grid polyurethane fluorescent optical imitation with the same IR-125 concentration and different fluorescent sensitivity imitation depths.
FIG. 5 is a schematic diagram of a 9-grid polyurethane fluorescent optical imitation of the same IR-125 concentration and different fluorescent sensitivity imitation diameters.
FIG. 6 is a schematic diagram of polyurethane fluorescent optical imitations with 9 lattices of the same IR-125 concentration and different depths without fluorescent dye doping on the fluorescent sensitivity imitations.
Detailed Description
Reference will now be made in detail to exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, the same numbers in different drawings refer to the same or similar elements, unless otherwise indicated. The implementations described in the following exemplary examples do not represent all implementations consistent with the application.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any or all possible combinations of one or more of the associated listed items.
It should be understood that although the terms first, second, third, etc. may be used herein to describe various information, these information should not be limited by these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the application. The word "if" as used herein may be interpreted as "at … …" or "at … …" or "in response to a determination" depending on the context.
The polyurethane fluorescent optical imitation body is in a multi-grid structure, and fluorescent imitation bodies are arranged in each unit grid of the multi-grid; the concentration of the fluorescent dye in the fluorescent imitation bodies in different unit cells changes in a gradient manner; or, the concentrations of the fluorescent dyes in the fluorescent simulants in different unit cells are the same, and the depth of the fluorescent simulants, the diameter of the fluorescent simulants or the depth of the simulants with the same depth, which are not doped with the fluorescent dyes and have scattering coefficients and absorption coefficients, are changed in a gradient manner; all fluorescent mimics of Gong Gezhong constitute fluorescent sensitivity mimics;
The preparation process of the fluorescence sensitivity imitation comprises the following steps:
Heating the polyurethane curing agent and the polyurethane prepolymer at high temperature in a vacuum state respectively to remove water; uniformly mixing the fluorescent dye, the polyurethane curing agent and the polyurethane prepolymer in a preset proportion, adding the mixture into a cell, and curing after air bubble pumping.
The fluorescence sensitivity imitations can be distributed in multiple lattices such as four lattices, six lattices, nine lattices, twelve lattices, twenty four lattices and the like, and the multiple lattices can be obtained by 3D printing.
Specifically, for fluorescent sensitivity imitators in which the concentration of fluorescent dye in the fluorescent imitators in different cells is changed in a gradient, the preparation process comprises:
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution respectively in a vacuum state to remove the water in the polyurethane prepolymer and the polyurethane cross-linking agent;
uniformly mixing fluorescent dyes with different masses with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring into different cells in a multi-grid, wherein the concentration of the fluorescent dye in the fluorescent imitation in each cell is in gradient change, the depth is the same and the diameter is the same, and extracting bubbles for curing.
Specifically, the fluorescent sensitivity imitators with the same concentration of fluorescent dye and gradient change of depth of the fluorescent imitators in different unit cells are prepared by the following steps:
Adding a scattering medium and an absorption medium into the polyurethane crosslinking agent, and fully and uniformly stirring to obtain a polyurethane crosslinking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution added with the scattering medium and the absorption medium in a vacuum state respectively to remove the moisture in the polyurethane prepolymer and the polyurethane cross-linking agent;
Uniformly mixing fluorescent dye with the same mass with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring the mixture into different cells in a multi-grid, wherein the pouring depth of each cell is in gradient change, the fluorescence concentration is the same, the diameter is the same, and curing is performed after air bubbles are extracted.
Specifically, for a fluorescence sensitivity imitation body which has no fluorescent dye doping on the same-depth fluorescence imitation body and has gradient change of depth of imitation body with scattering coefficient and absorption coefficient, two layers are divided into each cell, and the lower layer is a fluorescence imitation body with the same fluorescent dye concentration, the same depth and the same diameter in different cells; the upper layer is a non-fluorescent imitation body which does not contain fluorescent dye, contains scattering property and absorption property and has gradient change of depth in different cells, and the fluorescent imitation bodies in all the cells jointly form a depth sensitivity imitation body, and the preparation process comprises the following steps:
Adding a scattering medium and an absorption medium into the polyurethane crosslinking agent, and fully and uniformly stirring to obtain a polyurethane crosslinking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution added with the scattering medium and the absorption medium in a vacuum state respectively to remove the moisture in the polyurethane prepolymer and the polyurethane cross-linking agent;
uniformly mixing fluorescent dye with the same mass with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring the mixed solution and polyurethane prepolymer into different cells in a multi-grid, pouring the mixed solution and polyurethane prepolymer into each cell with the same depth and diameter, extracting bubbles and curing;
The polyurethane cross-linking agent mixed solution and the polyurethane prepolymer with corresponding proportions are uniformly mixed and respectively poured into different cells in the multi-cell, the pouring depth of each cell is in gradient change and the diameter is the same, and the cells are solidified after being extracted, wherein the scattering coefficient and the absorption coefficient of an imitation body formed by twice solidification in each cell are the same.
Specifically, the fluorescent imitators with the same fluorescent dye concentration and gradient change of fluorescent sensitivity imitators diameter in different unit cells are prepared by the following steps:
Adding a scattering medium and an absorption medium into the polyurethane crosslinking agent, and fully and uniformly stirring to obtain a polyurethane crosslinking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution added with the scattering medium and the absorption medium in a vacuum state respectively to remove the moisture in the polyurethane prepolymer and the polyurethane cross-linking agent;
uniformly mixing fluorescent dyes with the same mass with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring the mixed solution and polyurethane prepolymer into different cells in a multi-cell grid, extracting bubbles, and solidifying, wherein the diameter of each cell is in gradient change, and the concentration and depth of the fluorescent dyes are the same.
Specifically, the fluorescent sensitivity imitators with the same scattering coefficient and gradient change of the concentration of fluorescent dye in the fluorescent imitators in different unit cells are prepared by the following steps:
Adding scattering media with the same mass into a plurality of polyurethane cross-linking agents, and fully and uniformly stirring to form polyurethane cross-linking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution respectively in a vacuum state to remove the water in the polyurethane prepolymer and the polyurethane cross-linking agent;
Uniformly mixing fluorescent dye with gradient change quality with polyurethane prepolymer and polyurethane cross-linking agent mixed solution in a preset proportion, respectively pouring the mixture into different cells of a multi-cell grid, and extracting bubbles for solidification, wherein the concentration of the dye poured into each cell grid is gradient change, the depth is the same, and the diameter is the same.
Specifically, the fluorescent sensitivity imitators with gradient change of the concentration of fluorescent dye in the fluorescent imitators in different cells and same scattering coefficient and absorption coefficient are prepared by the following steps:
respectively adding scattering medium and absorption medium with the same mass into a plurality of polyurethane cross-linking agents, and fully and uniformly stirring to form polyurethane cross-linking agent mixed solution;
respectively heating polyurethane prepolymer and polyurethane cross-linking agent mixed solution with gradient change of absorption medium concentration in vacuum state to remove water in polyurethane prepolymer and polyurethane cross-linking agent;
Uniformly mixing fluorescent dye with gradient mass and polyurethane prepolymer and polyurethane cross-linking agent mixed solution in a preset proportion, respectively pouring the mixed solution into different cells of the multi-cell, and extracting bubbles for curing.
The application does not limit the kind of fluorescent dye. Examples of the fluorescent dyes are nine-bar and IR-125.
In one embodiment, a method for producing a polyurethane fluorescent optical imitation having a gradient concentration comprises:
respectively heating the polyurethane prepolymer and the polyurethane curing agent at a high temperature in a vacuum state to remove water in the polyurethane prepolymer and the polyurethane curing agent;
In the high-temperature heating process, weighing IR-125 fluorescent dyes with various masses by using a balance, respectively filling the IR-125 fluorescent dyes into sample bottles, namely bottles I, II, III, … and N, wherein the concentrations of the IR-125 in the N bottles are in gradient change (in one embodiment, the concentration gradient is randomly and regularly set in 0.5 nmol/g-500 nmol/g), sucking a proper amount of ultra-dry dimethyl sulfoxide D3850 solution by using a needle tube, dripping the ultra-dry dimethyl sulfoxide D3850 solution into the bottles, and sequentially and completely dissolving the IR-125 fluorescent dyes in the N bottles;
sequentially pouring a certain amount (such as 10 g) of polyurethane curing agent and polyurethane prepolymer into a bottle I filled with and dissolved in IR-125, uniformly stirring, pouring into a nine-square lattice, placing into a bubble extraction box, and extracting bubbles in the nine-square lattice;
Then pouring a certain amount of polyurethane curing agent and Part A into a bottle II with different IR-125 amounts, uniformly stirring, pouring into a nine-grid, and placing into a bubble extraction box to extract bubbles;
then pouring a certain amount of polyurethane curing agent and polyurethane prepolymer into a bottle III filled with different IR-125 amounts, uniformly stirring, pouring into a nine-square lattice, and extracting bubbles in polyurethane in the nine-square lattice;
all remaining polyurethane mixtures of different IR-125 concentrations were poured into a nine-grid and air bubbles were extracted and cured at room temperature.
The above is the preparation of polyurethane fluorescent optical imitation with gradient concentration, and the obtained imitation is shown in figure 1, and can be used for calibrating the concentration sensitivity of an imaging system to fluorescent dye.
The curing time is determined by the ratio between the polyurethane prepolymer and the polyurethane cross-linking agent and the curing environment, the larger the ratio between the polyurethane cross-linking agent and the polyurethane prepolymer is, the longer the curing time of the polyurethane mixed solution is, the smaller the ratio between the polyurethane cross-linking agent and the polyurethane prepolymer is, the shorter the curing time of the polyurethane mixed solution is, and the preparation of the high-quality film can be realized by adjusting the ratio, and the ratio between the polyurethane prepolymer and the polyurethane cross-linking agent is generally set to be 1:2-2:1 based on the condition that the extraction bubbles are prevented from being influenced by too fast curing, and meanwhile, the too slow curing is prevented from prolonging the experimental duration.
For the other polyurethane fluorescent optical imitation body with the same depth and scattering coefficient of the nine squares and the gradient change of the IR-125 concentration. Unlike the preparation of the polyurethane fluorescent optical imitation with the gradient concentration, a certain amount of scattering material is doped in the polyurethane curing agent. The IR-125 concentration of each cell in the nine squares is changed in a gradient, and the concentration of the scattering material is unchanged. The obtained imitation body is shown in fig. 2, and can calibrate the concentration sensitivity of an imaging system to fluorescent dye under the condition of simulating human biological tissues.
Similarly, the other kind of polyurethane fluorescent optical imitation body with the same depth and the same absorption coefficient of the nine grids is prepared by gradient change of the concentration of IR-125. Unlike the production of the polyurethane fluorescent optical imitation with the gradient concentration, the polyurethane curing agent is doped with a certain amount of absorbing material. The IR-125 concentration of each cell in the nine grids is changed in a gradient manner, and the concentration of the absorbing material is unchanged. The resulting imitation is similar to fig. 2, in that it allows calibrating the concentration sensitivity of the imaging system for fluorescent dyes in case of simulating human biological tissue.
For the other polyurethane fluorescent optical imitation with the same IR-125 concentration, the same depth of the nine squares, the same scattering coefficient and the same absorption coefficient are produced in a gradient way. Unlike the preparation of the polyurethane fluorescent optical imitation with the gradient concentration, the polyurethane curing agent is doped with a certain amount of absorption medium and scattering medium. The IR-125 concentration of each cell in the multi-cell is changed in a gradient manner, and the concentration of the scattering material and the concentration of the absorption material are the same. The resulting imitation is shown in fig. 3, which calibrates the concentration sensitivity of the imaging system to the fluorescent dye in the case of more accurately simulating human biological tissue relative to the first two imitation.
For the other type of IR-125 concentration, the polyurethane fluorescent imitation body depth was changed in gradient, and the depth sensitivity imitation body with scattering property and absorption property was produced. Different from the preparation of the polyurethane fluorescent optical imitation with the gradient concentration, the quality of the IR-125 fluorescent dye in the bottle I, the bottle II, the bottle III and the bottle … is the same, the concentration of the IR-125 fluorescent dye in each unit cell in the nine grids is the same, and the depth presentation is increased and changed. The resulting imitation is shown in FIG. 4, and can be used to calibrate the volumetric sensitivity of an imaging system to fluorescent dyes.
For the other polyurethane fluorescent optical imitation with the same IR-125 concentration, the diameter of the cylinder is changed in a gradient way. Different from the preparation of the polyurethane fluorescent optical imitation with the gradient concentration, the quality of the IR-125 fluorescent dye in the bottle I, the bottle II, the bottle III and the bottle … is the same, the concentration of the IR-125 fluorescent dye in each unit cell in the nine grids is the same, and the diameter is presented and changed. The resulting imitation is shown in FIG. 5, and can be used to calibrate the area sensitivity of an imaging system to fluorescent dyes.
For the imaging depth sensitivity fluorescent imitation body with scattering property and absorption property, namely the IR-125 concentration is the same, the nine palace lattice depths are different, the scattering coefficient is the same, the absorption coefficient is the same, and the polyurethane fluorescent optical imitation body without the depth of the fluorescent dye doped imitation body on the fluorescent sensitivity imitation body is manufactured by two steps: the first step, the manufacturing method of the polyurethane fluorescent optical imitation body with the same IR-125 concentration and gradient change of depth is different from that of the other polyurethane fluorescent optical imitation body, wherein the pouring amount of each unit in the Jiugong lattice is the same (namely, the cylindrical depth is the same), and after the preparation and solidification are finished; and a second step of pouring a mixed solution of the polyurethane prepolymer and the polyurethane crosslinking agent which has the same scattering coefficient and the same absorption coefficient but does not contain IR-125, based on the first step, wherein the step is the same as the first step except that the pouring depth of each unit in the nine-square lattice is in an increasing trend. The lower cell of each cell in the nine grids has the same concentration of IR-125, the same scattering coefficient and absorption coefficient, and the same amount, and the upper cell of each cell has the same composition as the lower cell except that the upper cell does not contain IR-125, and the depth presents increased variation. The resulting imitation is shown in FIG. 6, and can be used to calibrate the imaging system's depth sensitivity to fluorescent dyes.
The method can be used for manufacturing the cylindrical fluorescent optical imitation bodies with multiple lattices and different concentrations, can also be used for manufacturing fluorescent optical imitation bodies with different depths, can also be used for manufacturing fluorescent optical imitation bodies with scattering coefficients and absorption coefficients, can be used for manufacturing fluorescent optical imitation bodies with different cylindrical diameters, and can also be combined with a spin coating technology to form the multifunctional polyurethane fluorescent optical imitation body through spin coating of multiple layers of films with different thicknesses. The addition of IR-125 to the polyurethane matrix can simulate the performance (sensitivity, illumination uniformity, fluorescence intensity) of a fluorescence imaging system, and the addition of the scattering material and the absorbing material can simulate the optical characteristics (refractive index, scattering coefficient, absorption coefficient, anisotropy factor) of biological tissues and the distribution of light in the simulated tissues, thereby being beneficial to the establishment and light path alignment of the fluorescence imaging system, the measurement of performance indexes, the performance calibration and the comparison of different fluorescence imaging systems. The imitation body with different concentrations can be manufactured, so that the sensitivity of a fluorescence system can be measured, and the difference of the lowest detectable concentration between different fluorescence imaging systems can be detected. The mold body with different depths can simulate the fluorescence intensity of the subcutis with different depths. The multi-layer polyurethane film with the scattering coefficient and the absorption coefficient is coated on the surface of the multi-grid with the multifunctional polyurethane fluorescent optical imitation body in a spin mode, the layered structure and the optical characteristic of tissues can be simulated, the fluorescent characteristic under the tissue structure can be calibrated, and the performance of optical coherence tomography can be measured and calibrated. The polyurethane fluorescent optical imitation body has the advantages of multiple functions, high precision, high yield and high repetition rate.
In addition, the multi-layer polyurethane/PDMS/polyester/PMMA films with different scattering coefficients and absorption coefficients are spin-coated on the surfaces of the multi-grid with the multifunctional polyurethane fluorescent optical imitation body, so that the layered structure and optical characteristics of tissues can be simulated, the fluorescent characteristics under the tissue structure can be calibrated, and the performance of optical coherence tomography can be measured and calibrated.
The scattering medium can be TiO 2 nano-particles, siO 2 nano-particles, al 2O3 nano-particles and the like; the absorption medium may be nano carbon powder, silicon nano powder, indian ink, etc. In the implementation, the absorption medium may be a fluorescent agent or a quantum dot, but the absorption center wavelength of the fluorescent agent or the quantum dot is staggered from the emission center wavelength of the fluorescent dye used by the fluorescent imitation body.
The thickness of the polyurethane fluorescent imitation body is adjustable and can be 0.1 mm-15 mm.
After vacuum high-temperature dehydration is carried out before the polyurethane prepolymer and the polyurethane crosslinking agent are mixed, the moisture content is controlled below 0.02%, and after the polyurethane prepolymer and the polyurethane crosslinking agent are mixed, an air bubble extraction instrument is used for extracting bubbles in the mixed solution.
The vacuum high temperature heating dehydration is carried out, the temperature is set to be 90 ℃ to 100 ℃ and the duration is 10 h to 36 h.
Before the polyurethane prepolymer and the polyurethane crosslinking agent are mixed, the temperature of the polyurethane prepolymer and the polyurethane crosslinking agent is controlled in a high temperature state to delay the curing.
The polyurethane fluorescent optical imitation body not only can simulate the fluorescent concentration sensitivity, the diameter sensitivity and the depth sensitivity of fluorescent imaging equipment, but also can simulate the layered structure of tissues, and can test the performance of an optical coherence tomography and fluorescent imaging system, including longitudinal resolution and imaging depth, and the emission spectrum and the emission intensity of fluorescent imaging. The performance of the optical coherence tomography system and the fluorescence imaging system (two-photon imaging, confocal, wide-field fluorescence imaging and multiphoton imaging) can be calibrated. The polyurethane fluorescent optical imitation body has the advantages of high repeatability of fluorescent concentration, scattering coefficient and absorption coefficient, high precision, high controllability, mass production and low cost, and can be used for calibrating imaging depth and longitudinal resolution of fluorescent optical imaging equipment, OCT imaging equipment and photoacoustic imaging equipment by combining high precision level with a spin coater.
Other embodiments of the application will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure herein. This application is intended to cover any variations, uses, or adaptations of the application following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the application pertains.
It is to be understood that the application is not limited to the precise arrangements and instrumentalities shown in the drawings, which have been described above, and that various modifications and changes may be effected without departing from the scope thereof.
Claims (10)
1. The polyurethane fluorescent optical imitation is characterized by being in a multi-grid structure, wherein each unit grid of the multi-grid is provided with a fluorescent imitation;
the concentration of the fluorescent dye in the fluorescent imitation bodies in different unit cells changes in a gradient manner; or alternatively, the first and second heat exchangers may be,
The concentrations of the fluorescent dyes in the fluorescent simulants in different unit cells are the same, and the depth of the fluorescent simulants, the diameter of the fluorescent simulants or the depth of the simulants with the same depth, which are not doped with the fluorescent dyes and have scattering coefficients and absorption coefficients, are changed in a gradient manner;
All fluorescent mimics of Gong Gezhong constitute fluorescent sensitivity mimics;
the preparation process of the fluorescent imitation comprises the following steps:
heating the polyurethane curing agent and the polyurethane prepolymer in a vacuum state respectively to remove water;
Uniformly mixing the fluorescent dye, the polyurethane curing agent and the polyurethane prepolymer in a preset proportion, adding the mixture into a cell, and curing after air bubble pumping.
2. The polyurethane fluorescent optical modifier of claim 1, wherein the fluorescent sensitivity modifier is prepared by a process comprising:
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution respectively in a vacuum state to remove the water in the polyurethane prepolymer and the polyurethane cross-linking agent;
uniformly mixing fluorescent dyes with different masses with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring into different cells in a multi-grid, wherein the concentration of the fluorescent dye in the fluorescent imitation in each cell is in gradient change, the depth is the same and the diameter is the same, and extracting bubbles for curing.
3. The polyurethane fluorescent optical modifier of claim 1, wherein the fluorescent modifier comprises fluorescent light-sensitive modifiers having the same concentration of fluorescent dye and gradient depth in the fluorescent modifier in different cells, and the preparation process comprises:
Adding a scattering medium and an absorption medium into the polyurethane crosslinking agent, and fully and uniformly stirring to obtain a polyurethane crosslinking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution added with the scattering medium and the absorption medium in a vacuum state respectively to remove the moisture in the polyurethane prepolymer and the polyurethane cross-linking agent;
Uniformly mixing fluorescent dye with the same mass with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring the mixture into different cells in a multi-grid, wherein the pouring depth of each cell is in gradient change, the fluorescence concentration is the same, the diameter is the same, and curing is performed after air bubbles are extracted.
4. The polyurethane fluorescent optical imitation of claim 1, wherein for a fluorescent imitation of the same depth, which is not doped with fluorescent dye and has a gradient change in depth of imitation of scattering coefficient and absorption coefficient, the fluorescent sensitivity imitation is divided into two layers in each cell, and the lower layer is a fluorescent imitation of the same concentration, depth and diameter of fluorescent dye in different cells; the upper layer is a non-fluorescent imitation body which does not contain fluorescent dye, contains scattering property and absorption property and has gradient change of depth in different cells, and the fluorescent imitation bodies in all the cells jointly form a depth sensitivity imitation body, and the preparation process comprises the following steps:
Adding a scattering medium and an absorption medium into the polyurethane crosslinking agent, and fully and uniformly stirring to obtain a polyurethane crosslinking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution added with the scattering medium and the absorption medium in a vacuum state respectively to remove the moisture in the polyurethane prepolymer and the polyurethane cross-linking agent;
uniformly mixing fluorescent dye with the same mass with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring the mixed solution and polyurethane prepolymer into different cells in a multi-grid, pouring the mixed solution and polyurethane prepolymer into each cell with the same depth and diameter, extracting bubbles and curing;
The polyurethane cross-linking agent mixed solution and the polyurethane prepolymer with corresponding proportions are uniformly mixed and respectively poured into different cells in the multi-cell, the pouring depth of each cell is in gradient change and the diameter is the same, and the cells are solidified after being extracted, wherein the scattering coefficient and the absorption coefficient of an imitation body formed by twice solidification in each cell are the same.
5. The polyurethane fluorescent optical imitation of claim 1, wherein the fluorescent dye concentration in the fluorescent imitation in different cells is the same, the fluorescent sensitivity imitation diameter is graded, the preparation process comprises:
Adding a scattering medium and an absorption medium into the polyurethane crosslinking agent, and fully and uniformly stirring to obtain a polyurethane crosslinking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution added with the scattering medium and the absorption medium in a vacuum state respectively to remove the moisture in the polyurethane prepolymer and the polyurethane cross-linking agent;
uniformly mixing fluorescent dyes with the same mass with polyurethane cross-linking agent mixed solution and polyurethane prepolymer in a preset proportion, respectively pouring the mixed solution and polyurethane prepolymer into different cells in a multi-cell grid, extracting bubbles, and solidifying, wherein the diameter of each cell is in gradient change, and the concentration and depth of the fluorescent dyes are the same.
6. The polyurethane fluorescent optical imitation of claim 1, wherein the fluorescent dye concentration in the fluorescent imitation in different cells is graded and the fluorescent sensitivity imitation with the same scattering coefficient is prepared by the following steps:
Adding scattering media with the same mass into a plurality of polyurethane cross-linking agents, and fully and uniformly stirring to form polyurethane cross-linking agent mixed solution;
heating the polyurethane prepolymer and the polyurethane cross-linking agent mixed solution respectively in a vacuum state to remove the water in the polyurethane prepolymer and the polyurethane cross-linking agent;
Uniformly mixing fluorescent dye with gradient change quality with polyurethane prepolymer and polyurethane cross-linking agent mixed solution in a preset proportion, respectively pouring the mixture into different cells of a multi-cell grid, and extracting bubbles for solidification, wherein the concentration of the dye poured into each cell grid is gradient change, the depth is the same, and the diameter is the same.
7. The polyurethane fluorescent optical imitation of claim 1, wherein the fluorescent dye concentration in the fluorescent imitation in different cells is a gradient, and the fluorescent sensitivity imitation with the same scattering coefficient and absorption coefficient is prepared by the following steps:
respectively adding scattering medium and absorption medium with the same mass into a plurality of polyurethane cross-linking agents, and fully and uniformly stirring to form polyurethane cross-linking agent mixed solution;
respectively heating polyurethane prepolymer and polyurethane cross-linking agent mixed solution with gradient change of absorption medium concentration in vacuum state to remove water in polyurethane prepolymer and polyurethane cross-linking agent;
Uniformly mixing fluorescent dye with gradient mass and polyurethane prepolymer and polyurethane cross-linking agent mixed solution in a preset proportion, respectively pouring the mixed solution into different cells of the multi-cell, and extracting bubbles for curing.
8. The polyurethane fluorescent optical imitation of claim 1, wherein: the ratio of the polyurethane prepolymer to the polyurethane crosslinking agent is 1:2-2:1.
9. The polyurethane fluorescent optical imitation of claim 1, wherein: heating and dehydrating under vacuum, setting 90-100 ℃ and duration 10 h-36 h;
after vacuum high-temperature dehydration is carried out before the polyurethane prepolymer and the polyurethane crosslinking agent are mixed, the moisture content is controlled below 0.02 percent, and after the polyurethane prepolymer and the polyurethane crosslinking agent are mixed, an air bubble extracting instrument is utilized to extract bubbles in the mixed solution;
curing is retarded by controlling the temperature of the polyurethane prepolymer and the polyurethane crosslinking agent prior to mixing them.
10. A fluorescent optical imitation, characterized in that: the polyurethane fluorescent optical imitation body is obtained by spin coating a plurality of films on the surface of a multi-grid of the polyurethane fluorescent optical imitation body according to any one of claims 1-9, wherein the thickness, the scattering coefficient and the absorption coefficient of each layer are different, and the film material is polyurethane, PDMS, polyester or PMMA.
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| CN115719023A (en) * | 2022-11-24 | 2023-02-28 | 之江实验室 | Optical fiber fluorescence bionic die body and generation method and application thereof |
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| US4965087A (en) * | 1982-12-07 | 1990-10-23 | Avl Ag | Method of making a sensor element for fluorescence-optical measurements |
| JP2012068691A (en) * | 2010-09-21 | 2012-04-05 | Denso Wave Inc | Optical information reading device |
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