CN108276527B - Hydrogel composite device for ionizing radiation dose measurement and preparation method thereof - Google Patents
Hydrogel composite device for ionizing radiation dose measurement and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of a hydrogel composite device for ionizing radiation dose measurement, which comprises the following steps: mixing acrylamide, an anionic monomer, a polycation matrix and a photoinitiator in water, removing oxygen in the mixed solution, then carrying out ultraviolet illumination polymerization, and irradiating for 1-30 minutes to obtain a prepolymer; and placing the thermoluminescent dosimeter on the surface of the prepolymer, and continuing to irradiate the prepolymer with ultraviolet light to ensure that the prepolymer is completely polymerized to form the hydrogel composite device for measuring the ionizing radiation dose. The invention also claims the hydrogel composite device for measuring the ionizing radiation dose prepared by the preparation method. The method of the invention tightly combines hydrogel with excellent mechanical property and adhesion property with TLD, and the device can be tightly adhered to the surface of skin, thereby realizing accurate measurement of ionizing radiation dose.
Description
Technical Field
The invention relates to the technical field of medical high polymer materials and ionizing radiation measurement, in particular to a hydrogel composite device for measuring ionizing radiation dose and a preparation method thereof.
Background
Tumors seriously jeopardize the health and survival of human beings, and as one of the main means of tumor treatment, the development of radiotherapy technology puts higher and higher requirements on the treatment accuracy. Especially for patients with head and neck, breast tumor and skin cancer, the detection of the ionizing radiation dose on the skin surface is helpful to confirm the actual distribution of the dose, avoid skin inflammation and side reaction caused by excessive radiation treatment dose, and help to improve the precision of radiation treatment plan and quality control thereof.
The thermoluminescent dosimeter (TLD) is a solid having a crystal structure, and contains impurities to cause lattice defects, when electrons on a valence band acquire ionizing radiation energy, the electrons jump to a conduction band, and if the TLD is heated, the electrons can return to the valence band again, and the energy given by the ionizing radiation is radiated in the form of visible light, so that the purpose of ionizing radiation dose measurement is achieved. The method is commonly used for measuring the ionizing radiation accumulated dose, has the characteristics of higher sensitivity and precision, low light/heat fading, wider dose linear response range, smaller volume and the like, and has wide application in the field of radiation diagnosis and treatment dose measurement. However, the current TLD has the following disadvantages when applied: due to factors such as human body surface motion caused by respiration and inherent dose distribution gradient, the ionizing radiation dose accuracy measured by a single TLD is low, and ionizing radiation dose distribution information in a large range cannot be obtained; direct application of a dense TLD to an elastic, uneven skin surface can cause discomfort and inflammation to the skin, and the tightness of application is low.
The hydrogel is a three-dimensional network structure polymer material with high water content, and the physical and chemical properties of the hydrogel have high similarity with human tissues. Due to its good biocompatibility, it has been widely used in the biomedical material field, such as hydrogel dressing, tissue engineering, drug sustained release carrier, etc. And the hydrogel-based composite device is also regarded as the first choice of materials such as the next generation flexible electronic material and intelligent wound dressing. The hydrogel can be attached to the surface of human skin, and can not cause discomfort and inflammation of the skin. At present, a hydrogel and TLD composite device does not exist, and the common hydrogel material has the defects of low mechanical strength and extensibility, weak adhesion capability and the like, and cannot be used as a carrier for adhering skin and TLD.
Disclosure of Invention
In order to solve the above-mentioned technical problems, it is an object of the present invention to provide a hydrogel composite device for ionizing radiation dose measurement, which closely combines a hydrogel having excellent mechanical properties and adhesive properties with a TLD, and which can closely adhere to the surface of the skin, thereby achieving accurate measurement of the ionizing radiation dose, and a method for manufacturing the same.
In one aspect, the present invention provides a method of making a hydrogel composite device for ionizing radiation dose measurement, comprising the steps of:
(1) mixing acrylamide (AAm), an anionic monomer, a polycation matrix and a photoinitiator in water, removing oxygen in the mixed solution, then carrying out ultraviolet illumination polymerization, and irradiating for 1-30 minutes to obtain a prepolymer; preferably, between irradiation is 10-15 minutes;
(2) and (3) placing the TLD on the surface of the prepolymer, and continuing to irradiate the TLD with ultraviolet light to ensure that the prepolymer is completely polymerized to form the hydrogel composite device for measuring ionizing radiation dose.
Further, in the step (1), the concentration of acrylamide in the mixed solution is 0.5 to 5mol/L, the concentration of the anionic monomer in the mixed solution is 0.1 to 1mol/L, and the concentration of the polycation base in the mixed solution is 0.1 to 1 mol/L.
Preferably, the concentration of acrylamide in the mixed solution is 2 to 3mol/L, the concentration of the anionic monomer in the mixed solution is 0.2 to 0.4mol/L, and the concentration of the polycation matrix in the mixed solution is 0.2 to 0.4 mol/L.
Further, in the step (1), the anionic monomer is selected from one or more of acrylic acid (AAc), methacrylic acid, methyl butenoic acid and maleic acid.
Further, in the step (1), the polycation base is selected from one or more of polydiallyl dimethyl ammonium chloride (PDADMAC), polyethyleneimine, polylysine, polyethylene diamine and poly-2- (dimethylamino) ethyl methacrylate.
Further, in step (1), the anionic monomer is acrylic acid and the polycationic substrate is polydiallyldimethylammonium chloride.
Further, in the step (1), the concentration of the photoinitiator in the mixed solution was 2.3X 10-3-2.3×10-2mol/L. Preferably, the concentration of the photoinitiator in the mixed solution is 2.3X 10-3mol/L。
Further, in the step (1), the photoinitiator is 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone (Irgacure2959), 2-hydroxy-2, 2-dimethyl acetophenone or 2-hydroxy-2-methyl-1-phenyl-1-propanone. Preferably, the photoinitiator is Irgacure 2959.
Further, in the step (1), nitrogen gas is introduced into the mixed solution under the ultrasonic oscillation condition to remove oxygen therein.
Further, the nitrogen gas was introduced for 5 to 60 minutes. Preferably, the time of passage is 40 to 60 minutes.
Further, in the step (1) and the step (2), the intensity of ultraviolet irradiation is 3-20mW/cm2. Preferably, the intensity of ultraviolet irradiation is 8-10mW/cm2。
Further, in the step (2), the thermoluminescent dosimeter is selected from a lithium fluoride thermoluminescent dosimeter, a lithium borate thermoluminescent dosimeter, a calcium sulfate thermoluminescent dosimeter or a calcium fluoride thermoluminescent dosimeter.
Further, in the step (2), the light irradiation is continued for 30 to 60 minutes. Preferably, the illumination is continued for 50-60 minutes.
Further, in the step (2), the number of TLDs to be placed is 1 to plural. When multiple TLDs are placed, a TLD array is formed in the hydrogel, and a hydrogel-TLD array composite device is finally obtained.
The invention uses the interaction of hydrogen bond and positive and negative charges as a cross-linking point to construct a hydrogel material with high extensibility and high adhesion, and the hydrogel material has excellent mechanical property and adhesion property. The hydrogel material has the advantages that the polymer chain segments forming the hydrogel can be tightly combined through the hydrogen bond interaction between acrylamide and the anionic copolymer chain segments and the positive and negative charge interaction between the anionic chain segments and the polycation matrix, so that the mechanical property of the hydrogel is improved, the hydrogel can effectively dissipate energy during stretching, and the purpose of no fracture after stretching for a long distance is achieved.
The hydrogel matrix has polar groups, positive and negative charges, hydrogen bonds and the like, so that the hydrogel has excellent adhesion performance with the surfaces of various materials. Meanwhile, the hydrogel and the pyroelectric piece can form an interpenetrating network structure, so that the adhesion performance of the hydrogel and the pyroelectric piece is further improved. The TLD for radiation dose measurement is introduced in the hydrogel prepolymerization stage, and after polymerization to form the hydrogel, the TLD is wrapped on the surface of the hydrogel by a three-dimensional network of the polymer. The hydrogel carrier of the invention has high adhesiveness, can be tightly adhered to the surface of the skin, can tightly combine the skin and the TLD together, and overcomes the defects of low adhesion, discomfort and inflammatory reaction when the TLD is directly adhered to the skin. In another aspect, the present invention also provides a hydrogel composite device for ionizing radiation dosimetry prepared by the above-described preparation method.
By the scheme, the invention at least has the following advantages:
the hydrogel material with excellent mechanical property and adhesion property is closely combined with the TLD, has high extensibility and adhesion, is non-toxic and good in biocompatibility, is simple in preparation method, and overcomes the defects of poor extensibility, low adhesion, poor mechanical strength and the like of the common hydrogel. Meanwhile, the hydrogel composite device solves the problems that the TLD is easy to cause discomfort and skin inflammation in the modes of an adhesive tape and the like, solves the defect that devices such as a compact TLD and the like cannot be tightly adhered to the surface of the skin, retains the radiation dose measurement performance of the TLD, and can accurately measure the size and distribution of ionizing radiation irradiation dose on the surface of a human body in the radiotherapy process.
The hydrogel composite device designed by the invention tightly adheres the dose measuring equipment of the thermoluminescent dosimeter (TLD) to the surface of the skin of a human body, so that the measurement of the ionizing radiation dose on the surface of the skin of the human body in the radiotherapy process is realized. The TLD dose measurement function is well preserved, and the hydrogel composite device still has high sensitivity and accuracy, so that the measurement of the skin surface dose in the radiotherapy process is more accurate, and the error is reduced.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a stress-strain curve of hydrogel tension at different AAm concentrations, different cation concentrations, and different molar ratios of cations to anions according to the present invention;
FIG. 2 is a schematic diagram and physical representation of the structure of a hydrogel composite device of the invention;
FIG. 3 is a photograph of a hydrogel composite device according to the present invention in physical form before and after stretching;
FIG. 4 is a plot of the linear responsivity of TLDs and hydrogel composite devices of the present invention measured for ionizing radiation dose and dose rate under different dose rate irradiation;
FIG. 5 is a schematic representation of a hydrogel composite device illuminated at different radiation angles and the ability to measure dose under different radiation angles;
FIG. 6 is a schematic diagram of the structure of a hydrogel-TLD array composite device;
figure 7 is a graph of the measured dose data for a hydrogel-TLD array composite device irradiated at different degrees of flexure.
Description of reference numerals:
1-a hydrogel; 2-TLD.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
Mixing 70mmol AAm, 12mmol AAc and 12mmol PDADMAC, dissolving in 30mL deionized water, adding 0.07mmol photoinitiator Irgacure2959 into the mixed solution, ultrasonically oscillating and introducing nitrogen for 40 min to remove oxygen dissolved in the solution, sealing the mixed solution, and irradiating in front of an ultraviolet light source at an irradiation intensity of 8.5mW/cm2And after the irradiation is carried out for 10 minutes, the lithium fluoride thermoluminescence dosimeter is quickly and lightly placed on the surface of the prepolymer, so that the lithium fluoride thermoluminescence dosimeter is naturally soaked and floats on the surface, and the irradiation is continuously carried out for 60 minutes at the same light intensity, so that the hydrogel composite device for ionizing radiation dose measurement is obtained.
Example 2
A hydrogel composite device was prepared in the same manner as in example 1, except that AAm was used in an amount of 40 mmol.
Example 3
A hydrogel composite device was prepared in the same manner as in example 1, except that AAm was used in an amount of 50 mmol.
Example 4
A hydrogel composite device was prepared in the same manner as in example 1, except that AAm was used in an amount of 60 mmol.
Example 5
A hydrogel composite device was prepared in the same manner as in example 1, except that AAm was used in an amount of 80 mmol.
Example 6
A hydrogel composite device was prepared in the same manner as in example 1, except that AAm was used in an amount of 90 mmol.
Example 7
A hydrogel composite device was prepared in the same manner as in example 1, except that AAc was used in an amount of 2mmol, and PDADMAC was used in an amount of 2 mmol.
Example 8
A hydrogel composite device was prepared in the same manner as in example 1, except that AAc was used in an amount of 7mmol and PDADMAC was used in an amount of 7 mmol.
Example 9
A hydrogel composite device was prepared in the same manner as in example 1, except that AAc was used in an amount of 17mmol, and PDADMAC was used in an amount of 17 mmol.
Example 10
A hydrogel composite device was prepared in the same manner as in example 1, except that AAc was used in an amount of 22mmol, and PDADMAC was used in an amount of 22 mmol.
Example 11
A hydrogel composite device was prepared in the same manner as in example 1, except that AAc was used in an amount of 2.4mmol and PDADMAC was used in an amount of 21.6 mmol.
Example 12
A hydrogel composite device was produced in the same manner as in example 1, except that AAc was used in an amount of 7.2mmol and PDADMAC was used in an amount of 16.8 mmol.
Example 13
A hydrogel composite device was produced in the same manner as in example 1, except that AAc was used in an amount of 16.8mmol and PDADMAC was used in an amount of 7.2 mmol.
Example 14
A hydrogel composite device was prepared in the same manner as in example 1, except that AAc was used in an amount of 21.6mmol and PDADMAC was used in an amount of 2.4 mmol. FIG. 1 is a stress-strain curve of hydrogel tension at different AAm concentrations, different cation concentrations, and different molar ratios of cations to anions in the above examples.
PA in FIG. 1(a)xA12D12The expression means that the hydrogel composite device prepared by changing the concentration of AAm by selecting the dosage of 12mmol AAc and 12mmol PDADMAC, wherein x represents the dosage of AAm of 40mmol, 50mmol, 60mmol, 70mmol, 80mmol and 90mmol respectively. As can be seen, the strength at break and the elongation at break of the hydrogel increased with increasing AAm dosage.
PA in FIG. 1(b)70AyDzThe meaning of this is that 70mmol of AAm is selected, the amount of AAc and PDADMAC is changed to prepare a hydrogel composite device, the molar ratio of AAc to PDADMAC is 1:1, and the value of y in the figure represents the amount of AAc to be 2mmol, 7mmol, 12mmol, 17mmol and 22mmol, respectively. As can be seen, the strength at break of the hydrogel increases and the elongation at break decreases with increasing amounts of AAc and PDADMAC.
PA in FIG. 1(c)70AyDzThe meaning is that 70mmol AAm is selected, the amount of AAc and PDADMAC is changed, the sum of the mole numbers of the AAc and the PDADMAC is 24mmol, and y: z is 1:9, 3:7, 5:5, 7:3 and 9:1 respectively. As can be seen from the figure, as the molar ratio of the anions to the cations increases, the breaking strength of the hydrogel decreases and the elongation at break increases.
FIG. 2 is a schematic structural view and a physical diagram of a hydrogel composite device of the present invention, in FIG. 2(a), 1 represents a hydrogel; 2 represents TLD, which is seen from FIG. 2(c) to be very tightly bound to the hydrogel.
Figure 3 is a diagram of the physical state of the hydrogel composite device before and after 400% stretching, with the TLD still tightly bound to the hydrogel at 4 times stretching.
Fig. 4(a) is the linear responsivity of a pure TLD and a hydrogel composite device to ionizing radiation dose measurement, fig. 4(b) is the dose rate independence of the pure TLD and the hydrogel composite device under irradiation at different dose rates, fig. 4 shows that the accumulated dose measurement functions of the pure TLD and the hydrogel composite device are not affected by different dose rates, and the capability of the hydrogel composite device of the present invention for measuring dose is much higher than that of the pure TLD.
Fig. 5(a) illustrates a schematic view of a composite device under different radiation angles, which are 30 degrees, 60 degrees and 90 degrees, respectively. Figure 5(b) illustrates the ability of a pure TLD and a hydrogel composite device to measure dose under different radiation angles, demonstrating that both measure ionizing radiation with an angle dependence and that the hydrogel composite device of the present invention has much higher dose measurement ability than a pure TLD.
Example 15
Mixing 70mmol AAm, 12mmol maleic acid and 12mmol polylysine, dissolving in 30mL deionized water, adding 0.07mmol photoinitiator 2-hydroxy-2, 2-dimethyl acetophenone into the mixed solution, ultrasonically oscillating and introducing nitrogen for 60 min to remove oxygen dissolved in the solution, sealing the mixed solution, and irradiating with 3mW/cm ultraviolet light source2And after 30 minutes of irradiation, the calcium sulfate thermoluminescence dosimeter is quickly and lightly placed on the surface of the prepolymer, so that the calcium sulfate thermoluminescence dosimeter is naturally soaked and floats on the surface, and after the calcium sulfate thermoluminescence dosimeter is continuously irradiated for 30 minutes at the same light intensity, the hydrogel composite device for ionizing radiation dose measurement is obtained.
Example 16
Mixing 70mmol AAm, 12mmol methyl butenoic acid and 12mmol poly 2- (dimethylamino) ethyl methacrylate, dissolving in 30mL deionized water, adding 0.07mmol photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-acetone into the mixed solution, ultrasonically oscillating and introducing nitrogen for 10 min to remove oxygen dissolved in the solution, sealing the mixed solution, and irradiating with 20mW/cm ultraviolet light2After 5 minutes of irradiation, the lithium borate thermoluminescent dosimeter is quickly and lightly placed on the surface of the prepolymer, so that the prepolymer is naturally soakedAfter the hydrogel composite device was floated on the surface and continuously irradiated with the same light intensity for 40 minutes, the hydrogel composite device for ionizing radiation dose measurement was obtained.
Example 17
A hydrogel composite device was prepared as in example 1, except that nine lithium fluoride thermoluminescent dosimeters were placed on the surface of the polymer to form a 3 × 3 array, and a hydrogel-TLD array composite device was formed after polymerization (fig. 6).
When the hydrogel-TLD array composite device is irradiated with radiation in a planar state (fig. 7(a)) and under different bending degrees (fig. 7(b) and 7(c)), it can be seen that in the planar state, the relative dose measurement values of the TLDs at different positions of the hydrogel-TLD array composite device are all above 260mGy, the bending degree is changed, the relative dose measurement value of the TLD farther away from the light source is about 260mGy, and the relative dose measurement value of the TLD closer to the light source is between 300 and 500 mGy. The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A method of making a hydrogel composite device for ionizing radiation dosimetry comprising the steps of:
(1) mixing acrylamide, an anionic monomer, a polycation matrix and a photoinitiator in water, removing oxygen in the mixed solution, then carrying out ultraviolet illumination polymerization, and irradiating for 1-30 minutes to obtain a prepolymer; the anionic monomer is selected from one or more of acrylic acid, methacrylic acid, methyl crotonic acid and maleic acid; the polycation matrix is selected from one or more of poly-diallyl dimethyl ammonium chloride, polyethyleneimine, polylysine, polyethylene diamine and poly-2- (dimethylamino) ethyl methacrylate;
(2) and placing the thermoluminescent dosimeter on the surface of the prepolymer, and continuing to irradiate the thermoluminescent dosimeter with ultraviolet light to ensure that the prepolymer is completely polymerized to form the hydrogel composite device for measuring the ionizing radiation dose.
2. The method of claim 1, wherein: in the step (1), the concentration of the acrylamide in the mixed solution is 0.5-5mol/L, the concentration of the anionic monomer in the mixed solution is 0.1-1mol/L, and the concentration of the polycation matrix in the mixed solution is 0.1-1 mol/L.
3. The method of claim 1, wherein: in step (1), the anionic monomer is acrylic acid and the polycationic substrate is polydiallyldimethylammonium chloride.
4. The method of claim 1, wherein: in the step (1), the concentration of the photoinitiator in the mixed solution is 2.3X 10-3-2.3×10-2mol/L。
5. The method of claim 1, wherein: in the step (1), the photoinitiator is 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone, 2-hydroxy-2, 2-dimethylacetophenone or 2-hydroxy-2-methyl-1-phenyl-1-propanone.
6. The method of claim 1, wherein: in the step (1) and the step (2), the intensity of ultraviolet irradiation is 3-20mW/cm2。
7. The method of claim 1, wherein: in the step (2), the thermoluminescent dosimeter is selected from a lithium fluoride thermoluminescent dosimeter, a lithium borate thermoluminescent dosimeter, a calcium sulfate thermoluminescent dosimeter or a calcium fluoride thermoluminescent dosimeter.
8. A hydrogel composite device for ionizing radiation dosimetry prepared by the preparation method of any one of claims 1 to 7.
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| CN110790949B (en) * | 2019-10-09 | 2021-03-16 | 天津工业大学 | Adhesive hydrogel and preparation method thereof |
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