CN108283731B - Nano mesoporous calcium phosphate particle coating on zirconia surface, preparation method and application thereof - Google Patents
Nano mesoporous calcium phosphate particle coating on zirconia surface, preparation method and application thereof Download PDFInfo
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/32—Phosphorus-containing materials, e.g. apatite
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/606—Coatings
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/62—Encapsulated active agents, e.g. emulsified droplets
- A61L2300/622—Microcapsules
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
Abstract
The invention provides a nano mesoporous calcium phosphate particle coating on the surface of zirconia, which comprises a zirconia sample body and a nano mesoporous calcium phosphate particle coating attached to the surface of the zirconia sample body, wherein the main components of the nano mesoporous calcium phosphate particle coating are calcium, magnesium, oxygen and phosphorus, the nano mesoporous calcium phosphate particle coating on the surface of the zirconia is mainly applied to the field of dental implant materials, the calcium phosphate coating doped with magnesium ions has chemical components closer to human bone tissues, and meanwhile, the nano mesoporous calcium phosphate particle coating enables the surface appearance of the zirconia to be more suitable for cell adhesion and migration. In addition, the mesoporous structure of the calcium phosphate particles can adsorb nutrient components required by cell adhesion proliferation such as serum and protein in the dental implant pit, and can also be used for pre-loading medicaments or bioactive components with special effects.
Description
Technical Field
The invention belongs to the technical field of biomedical materials, and particularly relates to a nano mesoporous calcium phosphate particle coating on the surface of zirconia, a preparation method and application thereof.
Background
One of the most commonly used restorative materials in zirconia dental treatment. In recent years, zirconia materials have been used for dental implants, particularly for the production of one-stage root implants, because of their advantages such as high mechanical strength and color close to natural dental tissue. In order to increase the osseointegration rate and effect of the implant after implantation, various surface coating techniques are widely used for the modification of the surface of the implant. The calcium phosphate material has chemical composition similar to that of human bone and tooth tissue, and can raise the biocompatibility of the implant, promote the early adhesion of bone cell and speed osseointegration. Meanwhile, compared with a smooth surface and an acid-etched rough surface, the nano-scale particle coating is more beneficial to migration and proliferation of cells, and a better osseointegration effect is realized. Ori Geuli et al, which is different from the nano mesoporous calcium phosphate coating on the surface of zirconia in the present invention, realizes the preparation of the hydroxyapatite coating on the surface of titanium by using an electrochemical deposition method.
Disclosure of Invention
In view of the above, the magnesium ion-doped nano-mesoporous calcium phosphate particles are prepared by a sedimentation method and uniformly coated on the surface of the zirconia material by an electrochemical method. The calcium phosphate coating doped with magnesium ions has chemical components closer to human bone tissues, and the surface appearance of the zirconium oxide is more suitable for cell adhesion and migration due to the nano particle coating. In addition, the mesoporous structure of the calcium phosphate particles can adsorb nutrient components required by cell adhesion proliferation such as serum and protein in the dental implant pit, and can also be used for pre-loading medicaments or bioactive components with special effects.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the nano mesoporous calcium phosphate particle coating on the surface of the zirconia comprises a zirconia sample body and the nano mesoporous calcium phosphate particle coating attached to the surface of the zirconia sample body, wherein the main components of the nano mesoporous calcium phosphate particle coating are calcium, magnesium, oxygen and phosphorus.
Preferably, the nano mesoporous calcium phosphate particle coating layer is composed of homogeneous calcium phosphate particles, wherein the calcium phosphate particles are spheres or ellipsoids with a mesoporous structure.
Preferably, the main functional groups of the calcium phosphate particles are phosphate and carbonate.
The invention also aims to provide a preparation method of the nano mesoporous calcium phosphate particle coating on the surface of the zirconia, which comprises the following steps:
A. preparation of nanoparticle dispersion solution:
adding prepared nano calcium phosphate particles with the mass volume fraction of 0.5% into a sodium citrate solution, oscillating and mixing, and then performing ultrasonic dispersion under the power of 100% amplitude to obtain a stably dispersed nano particle suspension;
B. pretreatment of the zirconia material:
(a) cutting the presintered zirconia into samples with regular sizes by using a precision cutting machine;
(b) polishing the zirconia samples obtained in the step (a) step by using sand paper with different particle sizes respectively;
(c) heating to 1200 ℃ by using a high-temperature resistance furnace, continuously sintering for 2 hours, and naturally cooling;
(d) polishing the sintered zirconia sample in the step (c) step by using sand paper with different particle sizes;
(e) ultrasonically washing the polished zirconium oxide sample obtained in the step (d) by using acetone, ethanol and deionized water respectively;
(f) naturally air-drying the zirconia sample, and carrying out acid etching on the sample by using a mixed solution of hydrofluoric acid and concentrated nitric acid;
(g) repeatedly ultrasonically cleaning the zirconium oxide sample by using ultrapure water, and naturally air-drying the zirconium oxide sample;
C. electrochemical sedimentation:
(a) adding a potassium nitrate solution into the nanoparticle dispersion liquid obtained in the step A, and uniformly stirring to obtain an electrolyte;
(b) taking a platinum wire electrode as an auxiliary electrode, a silver/silver chloride electrode as a reference electrode, and a zirconium oxide sample as a working electrode;
(c) applying working voltage to two ends of the electrode for more than 30 minutes to carry out electrochemical deposition;
(d) and after the electrochemical deposition is finished, repeatedly washing the zirconium oxide sample by using ultrapure water and naturally drying.
Preferably, the ultrasonic dispersion time in the step a is 15 minutes or more.
Preferably, the average heating rate of the high-temperature resistance furnace in the step B is 30 ℃/min.
Preferably, in the mixed solution in the step B, the volume ratio of the hydrofluoric acid to the concentrated nitric acid is 2% and 65%, wherein the mass fraction of the hydrofluoric acid is 40%, the mass fraction of the nitric acid is 65%, and the acid etching time is 3 minutes.
Preferably, the operating voltages applied in step C are 10V, 20V and 30V, respectively.
The invention also aims to provide an application of the nano mesoporous calcium phosphate particle coating on the surface of the zirconia in the field of dental implant materials.
Compared with the prior art, the nano mesoporous calcium phosphate particle coating prepared by the electrochemical sedimentation method has higher biocompatibility and richer modification potential for common commercial zirconia materials.
Specifically, the nano mesoporous calcium phosphate particle coating on the surface of the zirconia has the following advantages:
(1) preparing to obtain nano calcium phosphate particles with mesoporous structures, and realizing stable suspension dispersion of the nano calcium phosphate particles in a conductive solution through an organic acid solution;
(2) uniformly coating mesoporous nano calcium phosphate particles dispersed in a conductive solution on the surface of a zirconia material through an electrochemical reaction to form a stable nano mesoporous calcium phosphate particle coating;
(3) the surface chemical composition and morphology of the zirconia material are changed through the nano mesoporous calcium phosphate particle coating, and the adhesion and proliferation of bone cells are promoted.
Drawings
FIG. 1 is a transmission electron micrograph (scale: 20nm) of the nano calcium phosphate particles of example 1;
FIG. 2 is a scanning electron micrograph (scale: 500nm) of the nano calcium phosphate particles of example 1;
FIG. 3 is a Fourier transform infrared spectrum of the calcium phosphate nanoparticles of example 1;
FIG. 4 is an X-ray diffraction pattern of the nano calcium phosphate particles in example 1;
FIG. 5 is a graph of X-ray energy spectrum analysis of the nano calcium phosphate particles in example 1;
FIG. 6 is a scanning electron micrograph (scale: 50 μm) of the surface of the zirconia after grinding and polishing in example 1;
FIG. 7 is a high-power scanning electron micrograph (scale: 5 μm) of the surface of the zirconia after grinding and polishing in example 1;
FIG. 8 is an atomic force microscope photograph of the surface of the zirconia after grinding and polishing in example 1;
FIG. 9 is a scanning electron micrograph (scale: 50 μm) of the surface of zirconia after acid etching treatment in example 1;
FIG. 10 is a scanning electron micrograph (scale: 5 μm) of the surface of zirconia after acid etching treatment in example 1;
FIG. 11 is an atomic force microscope photograph of the surface of zirconia after acid etching treatment in example 1;
FIG. 12 is a scanning electron micrograph (scale: 50 μm) of the surface of the zirconia after the electrochemical coating treatment in example 1;
FIG. 13 is a scanning electron micrograph (scale: 5 μm) of the surface of the zirconia after the electrochemical coating treatment in example 1;
FIG. 14 is an atomic force microscope image of the surface of zirconia after electrochemical coating treatment in example 1;
FIG. 15 is a graph showing an X-ray energy spectrum analysis of the surface elements of zirconia in the cutting and polishing group in example 1;
FIG. 16 is a graph showing an X-ray energy spectrum analysis of the surface elements of zirconia in the acid etching treatment group in example 1;
FIG. 17 is a chart of X-ray energy spectrum analysis of the zirconia surface elements of the nanolayered coating set of example 1;
FIG. 18 shows the distribution of the nanoparticles prepared in example 1 in sodium citrate solutions of different pH values;
FIG. 19 shows the cell adhesion of the surface of the zirconium oxide treated with the coating layer of nano-sized mesoporous calcium phosphate particles prepared in example 1 (scale: 200 μm).
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to the following examples and accompanying drawings.
Example 1
Mixing 750mL of calcium chloride solution with 0.2mol/L and 250mL of magnesium chloride solution with 0.2mol/L, adding sodium dodecyl phosphate solution with 500mL of sodium dodecyl phosphate solution with 4.66mg/mL of the mixture, and stirring the mixture to uniformly mix the mixture completely; adding a diammonium hydrogen phosphate solution into the mixed solution, controlling the element molar ratio to be (Ca + Mg)/P to be 1.67, adjusting the pH value to be 10.0 by using 33% ammonia water, continuously stirring, keeping the temperature at 60 ℃ for 24 hours, and continuously adjusting the pH value during the constant temperature period to ensure that the pH value is not less than 10.0; and (3) centrifuging the liquid in the step to obtain nano particles, washing the nano particles with ultrapure water for 5 times, then washing the nano particles with absolute ethyl alcohol for 3 times, drying the obtained product at 120 ℃ for 24 hours, and storing the product in a dry environment to obtain the nano mesoporous calcium phosphate particles.
Preparation of nanoparticle dispersion solution:
adding 0.5% of the prepared nano calcium phosphate particles into a sodium citrate solution, oscillating, mixing, and performing ultrasonic dispersion for 20min at the amplitude power of 100% to obtain a stably dispersed nano particle suspension.
Pretreatment of the zirconia material:
cutting the presintered zirconia into samples with regular sizes by using a precision cutting machine; then, polishing the zirconium oxide samples step by using sand paper with different particle sizes respectively; heating to 1200 ℃ at an average heating rate of 30 ℃/min by using a high-temperature resistance furnace, continuously sintering for 2 hours, and then naturally cooling; polishing the sintered zirconia sample step by using abrasive paper with different particle sizes; then ultrasonically washing, grinding and polishing the polished zirconium oxide sample by using acetone, ethanol and deionized water respectively; naturally drying, and carrying out acid etching on the sample for 3 minutes by using a mixed solution of 40% hydrofluoric acid and 65% concentrated nitric acid (the volume ratio of the hydrofluoric acid to the concentrated nitric acid is 2% and 65%); then the zirconium oxide sample is naturally air-dried after the repeated ultrasonic cleaning by ultrapure water.
Electrochemical sedimentation:
adding a potassium nitrate solution into the nanoparticle suspension, uniformly stirring and mixing the solution to serve as an electrolyte, taking a platinum wire electrode as an auxiliary electrode, taking a silver/silver chloride electrode as a reference electrode, taking a zirconium oxide sample as a working electrode, and applying certain working voltages (10V, 20V and 30V respectively) to the two ends of the electrode for more than 30 minutes; and after the electrochemical deposition is finished, repeatedly washing the zirconium oxide sample by using ultrapure water and naturally drying.
It is apparent from fig. 1 and 2 that the prepared nanoparticles are homogeneous spheres or ellipsoids having a mesoporous structure; it can be seen from fig. 3 that the prepared nanoparticles contain a certain amount of carbonate and phosphate; comparing the X-ray diffraction pattern of FIG. 4 with that of a standard card (JCPDS card #09-0432), the main component of the prepared nanoparticles is Ca5(PO4)3(OH) hydroxyapatite; it can be seen from the X-ray energy spectrum analysis chart of fig. 5 that the main components of the nano mesoporous calcium phosphate particles are calcium, magnesium, oxygen and phosphorus.
TABLE 1 comparative analysis of surface roughness of zirconia samples after different treatments
TABLE 2 comparative analysis of elemental composition on the surface of zirconia samples after different treatments
Example 2
Mixing 750mL of calcium nitrate solution with 0.2mol/L of magnesium nitrate solution with 250mL of magnesium nitrate solution with 0.2mol/L of magnesium nitrate solution, adding sodium dodecyl phosphate solution with 500mL of sodium dodecyl phosphate solution with 4.66mg/mL of magnesium nitrate solution, and stirring to uniformly mix the calcium dodecyl phosphate solution and the magnesium dodecyl phosphate solution; adding sodium dihydrogen phosphate solution into the mixed solution, controlling the element molar ratio (Ca + Mg)/P to be 1.67, adjusting the pH value to be 10.7 by using 33% ammonia water, continuously stirring, keeping the temperature at 60 ℃ for 28 hours, and continuously adjusting the pH value during the constant temperature period to ensure that the pH value is not less than 10.0; and centrifuging the liquid in the step to obtain nano particles, washing the nano particles for 3 times by using ultrapure water, then washing the nano particles for 3 times by using absolute ethyl alcohol, drying the obtained product for 32 hours at 120 ℃, and storing the product in a dry environment. The subsequent preparation method was the same as in example 1.
Example 3
Mixing 750mL of calcium chloride solution with 0.2mol/L and 250mL of magnesium chloride solution with 0.2mol/L, adding sodium dodecyl phosphate solution with 500mL of sodium dodecyl phosphate solution with 4.66mg/mL of the mixture, and stirring the mixture to uniformly mix the mixture completely; adding potassium phosphate solution into the mixed solution, controlling the element molar ratio to be (Ca + Mg)/P to be 1.67, adjusting the pH value to be 11.0 by using 33% ammonia water, continuously stirring, keeping the temperature at 60 ℃ for 24 hours, and continuously adjusting the pH value during the constant temperature period to ensure that the pH value is not less than 10.0; and C, centrifuging the liquid in the step B to obtain nano particles, washing the nano particles with ultrapure water for 5 times, then washing the nano particles with absolute ethyl alcohol for 5 times, drying the obtained product at 120 ℃ for 30 hours, and storing the product in a dry environment. The subsequent preparation method was the same as in example 1.
Nanoparticle dispersion experiments:
(1) adding 0.5% of nanoparticles to 10 millimoles per liter of sodium citrate solution at different pH values;
(2) and (3) carrying out ultrasonic oscillation for 15 minutes at the amplitude power of 100%, placing the suspension in a cuvette, standing and continuously observing the sedimentation condition of the nanoparticles.
As a result, as shown in fig. 18, the dispersibility of the solution was relatively poor when the solution was peracid (pH 2) or overbased (pH 12).
Osteoblast adhesion experiment
(1) Placing a zirconium oxide sample with a nano mesoporous calcium phosphate particle coating in a 24-pore plate through irradiation sterilization;
(2) uniformly inoculating human bone marrow mesenchymal cells on the surface of a zirconia sample;
(3) incubating for ten hours in a cell culture box at 37 ℃, fixing cells by glutaraldehyde, dehydrating step by step, and freeze-drying;
(4) and observing the cell adhesion condition under a scanning electron microscope.
The results of the experiment are shown in FIG. 19.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A preparation method of a nano mesoporous calcium phosphate particle coating on the surface of zirconia is characterized by comprising the following steps: the method comprises the following steps:
A. preparation of nanoparticle dispersion solution:
adding prepared nano calcium phosphate particles with the mass volume fraction of 0.5% into a sodium citrate solution, oscillating and mixing, and then performing ultrasonic dispersion under the power of 100% amplitude for more than 15 minutes to obtain a stably dispersed nano particle suspension;
B. pretreatment of the zirconia material:
(a) cutting the presintered zirconia into samples with regular sizes by using a precision cutting machine;
(b) polishing the zirconia samples obtained in the step (a) step by using sand paper with different particle sizes respectively;
(c) heating to 1200 ℃ by using a high-temperature resistance furnace, continuously sintering for 2 hours, and naturally cooling;
(d) polishing the sintered zirconia sample in the step (c) step by using sand paper with different particle sizes;
(e) ultrasonically washing the polished zirconium oxide sample obtained in the step (d) by using acetone, ethanol and deionized water respectively;
(f) naturally air-drying the zirconia sample, and carrying out acid etching on the sample by using a mixed solution of hydrofluoric acid and concentrated nitric acid;
(g) repeatedly ultrasonically cleaning the zirconium oxide sample by using ultrapure water, and naturally air-drying the zirconium oxide sample;
C. electrochemical sedimentation:
(a) adding a potassium nitrate solution into the nanoparticle dispersion liquid obtained in the step A, and uniformly stirring to obtain an electrolyte;
(b) taking a platinum wire electrode as an auxiliary electrode, a silver/silver chloride electrode as a reference electrode, and a zirconium oxide sample as a working electrode;
(c) applying working voltage to two ends of the electrode for more than 30 minutes to carry out electrochemical deposition;
(d) repeatedly washing the zirconium oxide sample by using ultrapure water after the electrochemical deposition is finished and naturally drying;
the obtained nano mesoporous calcium phosphate particle coating on the surface of the zirconia comprises a zirconia sample body and the nano mesoporous calcium phosphate particle coating attached to the surface of the zirconia sample body, wherein the main components of the nano mesoporous calcium phosphate particle coating are calcium, magnesium, oxygen and phosphorus, the nano mesoporous calcium phosphate particle coating is composed of homogeneous calcium phosphate particles, the calcium phosphate particles are spheres or ellipsoids with mesoporous structures, and the main functional groups of the calcium phosphate particles are phosphate radicals and carbonate radicals.
2. The method of claim 1, wherein: and the average heating rate of the high-temperature resistance furnace in the step B is 30 ℃/min.
3. The method of claim 1, wherein: and B, the volume ratio of the hydrofluoric acid in the mixed solution in the step B is 2%, the volume ratio of the concentrated nitric acid is 65%, wherein the mass fraction of the hydrofluoric acid is 40%, the mass fraction of the nitric acid is 65%, and the acid etching time is 3 minutes.
4. The method of claim 1, wherein: the working voltage applied in the step C is 10V, 20V and 30V respectively.
5. The application of the nano mesoporous calcium phosphate particle coating on the surface of the zirconia prepared by the preparation method according to claim 1 in the field of dental implant materials.
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| JP2001231849A (en) * | 2000-02-24 | 2001-08-28 | Matsushita Electric Works Ltd | Calcium phosphate coated zirconia biomaterial and its preparation |
| CN101791436A (en) * | 2010-04-15 | 2010-08-04 | 四川大学 | Biomedical material with porous calcium phosphate-chitosan composite coating |
| CN103088383A (en) * | 2011-11-04 | 2013-05-08 | 电子科技大学 | Electrochemical method for preparing citric acid-hydroxyapatite/zirconia transition coating on surface of biomedical titanium |
| CN105854080A (en) * | 2016-04-29 | 2016-08-17 | 成都贝施美生物科技有限公司 | Zirconia dental implant surface treatment method |
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2017
- 2017-12-22 CN CN201711407242.2A patent/CN108283731B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001231849A (en) * | 2000-02-24 | 2001-08-28 | Matsushita Electric Works Ltd | Calcium phosphate coated zirconia biomaterial and its preparation |
| CN101791436A (en) * | 2010-04-15 | 2010-08-04 | 四川大学 | Biomedical material with porous calcium phosphate-chitosan composite coating |
| CN103088383A (en) * | 2011-11-04 | 2013-05-08 | 电子科技大学 | Electrochemical method for preparing citric acid-hydroxyapatite/zirconia transition coating on surface of biomedical titanium |
| CN105854080A (en) * | 2016-04-29 | 2016-08-17 | 成都贝施美生物科技有限公司 | Zirconia dental implant surface treatment method |
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| Title |
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| Effects of magnesium-substituted nanohydroxyapatite coating on implant Osseointegration;Zhao Shi-fang等;《CLINICAL ORAL IMPLANTS RESEARCH》;20130801;第24卷;论文第447摘要部分，第451页第5-11行 * |
| 磷酸钙陶瓷颗粒微纳米结构对蛋白吸附的影响;李波等;《高等学校化学学报》;20120310;第33卷(第3期);论文第34页Abstract部分，第35页Materials and methods部分 * |
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