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CN102557527B - Temperature control magnetic bone cement and preparation method thereof - Google Patents

Temperature control magnetic bone cement and preparation method thereof Download PDF

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Publication number
CN102557527B
CN102557527B CN 201210000742 CN201210000742A CN102557527B CN 102557527 B CN102557527 B CN 102557527B CN 201210000742 CN201210000742 CN 201210000742 CN 201210000742 A CN201210000742 A CN 201210000742A CN 102557527 B CN102557527 B CN 102557527B
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bone cement
temperature
zinc ferrite
manganese
preparation
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CN102557527A (en
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李光大
赵三团
胡志刚
马建华
乔晓岚
谢蟪旭
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Henan University of Science and Technology
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Henan University of Science and Technology
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Abstract

The invention relates to temperature control magnetic bone cement and a preparation method thereof. The preparation method comprises the following steps: weighing FeCl3 6H2O, ZnCl2 and MnCl2 4H2O, mixing the materials according to the stoichiometric ratio of Mn0.15Zn0.85Fe2O4, adding ultra-pure water for preparing a solution, reacting, then getting a precursor of a manganese-zinc ferrite, calcining the precursor of the manganese-zinc ferrite to get manganese-zinc ferrite powder, adding a spherical poly(methyl methacrylate) particle powder agent containing benzoyl peroxide into the manganese-zinc ferrite powder, uniformly mixing, further adding methyl methacrylate containing dimethyl mercaptopropionic acid, and blending to prepare a product. The Curie temperature of the bone cement prepared by the preparation method disclosed by the invention is about 50 DEG C, the magnetic bone cement containing the manganese-zinc ferrite in the different proportions can raise the temperature from 37 DEG C to 50 DEG C and be constant at the temperature under an external alternating magnetic field, and the temperature control performance is realized.

Description

A kind of temperature control magnetic bone cement and preparation method
Technical field
The present invention relates to a kind of bio-medical material, specifically a kind of temperature control magnetic bone cement and preparation method.
Background technology
The postoperative recurrence problem of bone tumor is a great problem of puzzlement medical circle.Bone tumor recurrence not only makes the patient stand more misery, but life-threatening very.Because the Problems Concerning Their Recurrence of bone tumor, people have proposed the requirement of oncotherapy function to the bone renovating material that originally only has bone repair and reconstruction function.Bone cement is a kind of by clinical widely used orthopaedics repair materials, and it is generally by solid phase and liquid-phase mixing, and having can clinical any figuration, handiness, the advantage such as performance is good.
The magnetic thermotherapy utilizes magnetisable material the externally-applied magnetic field power conversion can be become the characteristics of heat energy under alternating magnetic field, the suitable shape of magnetic induction dielectric material is implanted or is imported to patient's tumor locus, add suitable alternating magnetic field, can heat tumor area, (cancerous cell is will be dead more than 42 ℃ than normal cell and tissue characteristics more responsive to heat to utilize tumor cell and tissue, but and about normal cell heat resistanceheat resistant to 48 ℃), reach the purpose of high magnetic target therapy.Characteristics such as the magnetic induction thermotherapy has simple to operate, and is with low cost, safe, and side effect is little, and the magnetic induction medium is once implantation, thermotherapy repeatedly is so be particularly suitable for treating the bone tumor that is in the health depths.And the magnetic bone cement of exploitation tool is a hot research direction of bone material.
In magnetic thermotherapy process, the control of the temperature of area for treatment is most important.If heating-up temperature is crossed the low purpose that can not have thermotherapy, and if excess Temperature will be heated to normal tissue, cause the normal muscle in next door or neural etc. organize overheated necrosis.So when thermotherapy, realize the control of thermotherapy temperature, could be safety and the effectiveness of guaranteeing to treat.Wherein overheated is a phenomenon that must prevent.But the present magnetic bone cement material of studying does not nearly all design function of temperature control.In the reality use, just need to use other attemperating unit that temperature is carried out measurement and control, complex operation.
For magnetic material, can there be the Curie temperature characteristic, the magnetic of material disappears when temperature is higher than Curie temperature, and no longer can the magnetic induction heating.But the material that plays at present magnetic induction in the magnetic bone cement of exploitation almost is ferroso-ferric oxide entirely, although ferroso-ferric oxide has higher magnetic heat generation ability, but its Curie temperature is very high, has reached about 590 ℃, and the bone cement take ferroso-ferric oxide as the magnetic crystalline phase is very easy to superheated.
Summary of the invention
The present invention is for solving the existing easy superheated problem of magnetic bone cement, a kind of temperature control magnetic bone cement and preparation method thereof is provided, this bone cement has good cell compatibility, about 50 ℃ of Curie temperature, when temperature reached 50 ℃, material was stopped heating, and temperature can realize heating once again when being lower than this temperature, guarantee preference temperature, prevent from simultaneously in the thermotherapy process superheating phenomenon occuring, improve the safety of magnetic thermotherapy.
The present invention solves the problems of the technologies described above the technical scheme of employing to be: a kind of temperature control magnetic bone cement and preparation method comprise following steps:
One) preparation of manganese-zinc ferrite
1) takes by weighing respectively FeCl 36H 2O, ZnCl 2And MnCl 24H 2O also presses Mn 0.15Zn 0.85Fe 2O 4Stoichiometric proportion batching, add ultra-pure water, be made into the solution that concentration of metal ions is 0.3mol/L, under 90 ℃ constant temperature, react 4h;
In the course of reaction, the NaOH solution that drips concentration in the solution and be 1mol/L under the mixing speed of 3000rpm is take the pH value of control reaction solution as 10;
2) precipitation that produces after the reaction in the step 1 is washed and centrifugalize under the 6000rpm rotating speed with ultra-pure water, dry under the condition that is deposited in temperature 60 C, pressure 0.09-0.093MPa after the separation, obtain the manganese-zinc ferrite presoma, for subsequent use;
3) the manganese-zinc ferrite presoma that obtains is calcined 1h under the condition of 450 ℃ of temperature, pressure 0.09-0.093MPa, namely obtain manganese-zinc-ferrite powder;
Two) preparation of temperature control magnetic bone cement
4) preparation of bone cement substrate:
Get spherical poly methyl methacrylate particle powder, after screening, choose granularity less than the spherical poly methyl methacrylate particle powder of 200 purposes, then add therein benzoyl peroxide, mix homogeneously makes solid phase bone cement substrate, and is for subsequent use;
The mean molecule quantity of described spherical polymethyl methacrylate is 270kDa;
The addition of described benzoyl peroxide is 4 % of solid phase bone cement substrate gross weight;
Other gets methyl methacrylate monomer, makes liquid phase bone cement substrate after adding therein the dimethyl sulphoniopropionate mix homogeneously;
The addition of described dimethyl sulphoniopropionate is 2 % of liquid phase bone cement substrate gross weight;
5) get the manganese-zinc-ferrite powder that makes in the step 3 and join mix homogeneously in the bone cement solid-phase matrix in the step 4, make the bone cement compound; Then be that the ratio of 1:1 adds the bone cement liquid-phase substrate in the step 4 in the bone cement compound according to weight ratio, then use stainless steel knife to be in harmonious proportion 3min and namely make product;
Wherein, the addition of manganese-zinc-ferrite powder is the 40%-60% of final products gross weight.
Among the present invention, FeCl 36H 2O, ZnCl 2And MnCl 24H 2When O reacts, can cause the variation of pH in solution, therefore need to drip sodium hydroxide solution and make its pH value be stabilized in 10.
Among the present invention, the programming rate when the manganese-zinc ferrite presoma that makes is calcined is 5 ℃/min.
Beneficial effect: polymethyl methacrylate is present widely used bone cement clinically, and molecular formula is mixed in this research in polymethyl methacrylate be Mn 0.15Zn 0.85Fe 2O 4Manganese-zinc ferrite, but the preparation temperature control the magnetic bone cement.Studies show that this bone cement hardening time about 10-25min, meet clinically the requirement to bone cement curing operation time 8-30min; Comprcssive strength is about 83.6-98Mpa, and is approaching with the comprcssive strength of cortical bone; The MTT experiment shows that material has good cell compatibility; The Curie temperature test shows the about 50 ° of C of Curie temperature of material, all can realize being warmed up to 50 ° of C from 37 ° of C adding the magnetic bone cement that contains the different proportion manganese-zinc ferrite under the alternating magnetic field, and in time increase continue not to heat up, but constant in this temperature, has realized temperature-control performance.The experimentation of Akihiko Matsumine etc. shows, when the magnetic material temperature reaches 50 ° of C, can make the temperature on osseous tissue surface to reach about the effective 43 ° of C of thermotherapy, and organizing around can not making again simultaneously is influenced.It is similar to it that the material magnetic heat generation of this research detects magnetic field intensity, and the Curie temperature of material is about 50 ° of C, can have beneficial effect so the reply of the material of this research design realizes temperature-controlled heat treatment treatment bone tumor.
The specific embodiment
The present invention is further elaborated below in conjunction with specific embodiment.
Embodiment 1
A kind of temperature control magnetic bone cement, its preparation process is as follows:
One) preparation of manganese-zinc ferrite
1) takes by weighing respectively FeCl 36H 2O, ZnCl 2And MnCl 24H 2O also presses Mn 0.15Zn 0.85Fe 2O 4Stoichiometric proportion batching, add ultra-pure water, be made into the solution that concentration of metal ions is 0.3mol/L, under 90 ℃ constant temperature, react 4h;
In the course of reaction, the NaOH solution that drips concentration in the solution and be 1mol/L under the mixing speed of 3000rpm is take the pH value of control reaction solution as 10;
2) precipitation that produces after the reaction in the step 1 is washed and centrifugalize under the 6000rpm rotating speed with ultra-pure water, dry under the condition that is deposited in temperature 60 C, pressure 0.09-0.093MPa after the separation, obtain the manganese-zinc ferrite presoma, for subsequent use;
3) the manganese-zinc ferrite presoma that obtains is calcined 1h under the condition of 450 ℃ of temperature, pressure 0.09-0.093MPa, namely obtain manganese-zinc-ferrite powder;
Two) preparation of temperature control magnetic bone cement
4) preparation of bone cement substrate:
Get spherical poly methyl methacrylate particle powder, after screening, choose granularity less than the spherical poly methyl methacrylate particle powder of 200 purposes, then add therein benzoyl peroxide, mix homogeneously makes solid phase bone cement substrate, and is for subsequent use;
The mean molecule quantity of described spherical polymethyl methacrylate is 270kDa;
The addition of described benzoyl peroxide is 4 % of solid phase bone cement substrate gross weight;
Other gets methyl methacrylate monomer, makes liquid phase bone cement substrate after adding therein the dimethyl sulphoniopropionate mix homogeneously;
The addition of described dimethyl sulphoniopropionate is 2 % of liquid phase bone cement substrate gross weight;
5) get the manganese-zinc-ferrite powder that makes in the step 3 and join mix homogeneously in the bone cement solid-phase matrix in the step 4, make the bone cement compound; Then be that the ratio of 1:1 adds the bone cement liquid-phase substrate in the step 4 in the bone cement compound according to weight ratio, then use stainless steel knife to be in harmonious proportion 3min and namely make product;
Wherein, the addition of manganese-zinc-ferrite powder is 50% of final products gross weight.
Get the temperature control magnetic bone cement that makes, check its indices method as follows:
One, hardening time;
After getting solid phase powder and liquid phase stirring 3min, move in Ф 9 * 5mm mould, flatten, place relative humidity 100%, in 37 ℃ of calorstats, the 400N load is lower, with the needle point diameter rustless steel pinprick concrete column face that is 1mm, stop to move down to load and be the cement solidification time.Get 5 samples, average.
Two, comprcssive strength;
After getting solid phase powder and liquid phase stirring 3min, sample is made the smooth cylindric sample of Ф 4 * 8mm in two ends, until after the sample solidifies with its 37 ℃ of calorstats at relative humidity 100% in maintenance 72h, use SHIMADZU SES-1000 to test its comprcssive strength, load 900N, pressing speed 1mm/min.Choose 5 harmless samples, test its meansigma methods for every group.
Three, crystalline phase forms;
Material is worn into fine powder, adopt X crystalline phase diffractometer (X'Pert Pro MPD X, Philips) to detect its crystalline phase and form 0.06 °/s of scanning step.
Four, magnetic test and magnetic heating performance detect;
Material is worn into the pillar of 3 millimeters of long 6 millimeters, diameters, use vibrating specimen magnetometer (Lake shore7410) to detect its magnetic; Material is made the cylinder of Ф 9 * 9mm, before curing, insert glass-stem thermometer, after cured material is placed radio-frequency induction coil, frequency 100kHz, magnetic field size 25K Am -1, temperature of every 5min record is tested its in time heating curve under alternating magnetic field, observes its intensification ability.
Five, the mensuration of material Curie temperature;
Adopt falling temperature method to measure the Curie temperature of material.Sample is placed even cooling system, allow it respectively at the situation borehole cooling that adds magnetic field and do not add magnetic field, record the cooling curve of sample, 2 corresponding temperature-visualizeds of curve burble point are sample Curie temperature roughly.
Six, cytotoxicity test;
With material with 37 ° of C oxirane disinfections, again the mass volume ratio (mg/mL) of material with 200:1 added in the culture fluid of LG-DMEM, 37 ° of C are hatched 24 h, with above-mentioned suspension high speed centrifugation, supernatant is with the filter paper filtering sterilization of 0.22 um, hydrochloric acid solution with 0.1 M is adjusted pH value to 7.4 ± 0.5, and the lixiviating solution that obtains adds 10% FBS as initial lixiviating solution, the cell experiment after initial lixiviating solution is used for afterwards by 2 times of GM culture fluid dilutions; Get the most vigorous third generation cell ROS17/2.8(rat osteosarcoma cells of growth after the recovery) (density is 5 * 10 in the cell inoculation 4Individual/ml) in 24 well culture plates, the original culture fluid of sucking-off behind the 24 h cell attachments, lixiviating solution 200 uL that add corresponding dilution number replace, organize in contrast with the GM culture fluid, cell culture ld, behind 3d and the 5d, 1,3,5d respectively gets a culture plate and adds MTT solution (5mg/ml) 40 μ l, continues to cultivate 4h under 37 ° of C, stops cultivating, the careful suction abandoned culture supernatant in the hole, every hole adds 420 μ l DMSO, and vibration 10min fully dissolves crystal, draw in every hole liquid 200 μ l in 96 hole flat undersides, then select the 570nm wavelength, measure each hole absorbance at enzyme-linked immunosorbent assay instrument, the record result.Do 3 Duplicate Samples (P＜0.05).
Adopt said method to detect its performance to the temperature control magnetic bone cement that makes, the result is: be 12 ± 2min its hardening time, and mechanical strength is 98.1 ± 5.3Mpa, is expected to for weight bearing area bone repairing and treating; XRD studies show that the main component of material is polymethyl methacrylate and manganese-zinc ferrite; Use vibrating specimen magnetometer to record material 1.59 * 10 6Am -1Saturation magnetization be 2.96Am 2Kg -1The Curie temperature that falling temperature method records material is about 50 ° of C; At 100kHz, 25K Am -1Alternating magnetic field under can see that material has good intensification ability, on 37 ° of C basal temperatures, through about 25min, material can be realized the intensification of 13 ° of C, reaches about 50 ° of C, reach this temperature after, the temperature constant of material has embodied function of temperature control about 50 ° of C.Cell experiment shows that material has good cell compatibility.
Embodiment 2
The preparation of the preparation of manganese-zinc ferrite and bone cement substrate all as described in Example 1.
Get manganese-zinc-ferrite powder and join mix homogeneously in the bone cement solid-phase matrix, make the bone cement compound; Then be that the ratio of 1:1 adds the bone cement liquid-phase substrate in the bone cement compound according to weight ratio, then use stainless steel knife to be in harmonious proportion 3min and namely make product;
Wherein, the addition of manganese-zinc-ferrite powder is 40% of final products gross weight.
Adopt the experimental technique among the embodiment 1 to detect its performance to the temperature control magnetic bone cement that makes, the result is: recording its hardening time is 10 ± 1min, mechanics comprcssive strength 91.1 ± 3.7Mpa; Use vibrating specimen magnetometer to record material 1.59 * 10 6Am -1Saturation magnetization be 1.97Am 2Kg -1Under the basal temperature of 37 ° of C, under alternating magnetic field, can realize heating up, be stabilized at last about 50 ° of C; The MTT experiment shows that material has good cell compatibility.
Embodiment 3
The preparation of the preparation of manganese-zinc ferrite and bone cement substrate all as described in Example 1.
Get manganese-zinc-ferrite powder and join mix homogeneously in the bone cement solid-phase matrix, make the bone cement compound; Then be that the ratio of 1:1 adds the bone cement liquid-phase substrate in the bone cement compound according to weight ratio, then use stainless steel knife to be in harmonious proportion 3min and namely make product;
Wherein, the addition of manganese-zinc-ferrite powder is 60% of final products gross weight.
Adopt the experimental technique among the embodiment 1 to detect its performance to the temperature control magnetic bone cement that makes, the result is: recording its hardening time is 25 ± 2.5min, comprcssive strength 83.6 ± 4.2Mpa; Use vibrating specimen magnetometer to record material 1.59 * 10 6Am -1Saturation magnetization be 3.15Am 2Kg -1Under the basal temperature of 37 ° of C, under alternating magnetic field, can realize heating up, be stabilized at last about 50 ° of C; The MTT experiment shows that material has good cell compatibility.

Claims (1)

1.一种温控磁性骨水泥的制备方法，其特征在于，包含以下步骤： 1. a preparation method of temperature-controlled magnetic bone cement, is characterized in that, comprises the following steps: 一）锰锌铁氧体的制备 1) Preparation of manganese zinc ferrite 1）分别称取FeCl3·6H2O、ZnCl2和MnCl2·4H2O并按Mn0.15Zn0.85Fe2O4的化学计量比配料，加入超纯水，配成金属离子浓度为0.3mol/L的溶液，在90℃的恒温条件下反应4h； 1) Weigh FeCl 3 6H 2 O, ZnCl 2 and MnCl 2 4H 2 O respectively and mix according to the stoichiometric ratio of Mn 0.15 Zn 0.85 Fe 2 O 4 , add ultrapure water to make the metal ion concentration 0.3mol /L solution, reacted for 4 hours at a constant temperature of 90°C; 反应过程中，在3000rpm的搅拌速度下往溶液中滴加浓度为1mol/L的NaOH溶液以控制反应溶液的pH值为10； During the reaction, the NaOH solution with a concentration of 1mol/L was added dropwise to the solution at a stirring speed of 3000rpm to control the pH value of the reaction solution to be 10; 2）将步骤1中反应后产生的沉淀用超纯水洗涤并在6000rpm转速下离心分离，分离后的沉淀在温度60℃、压强0.09-0.093MPa的条件下烘干，得到锰锌铁氧体前驱体，备用； 2) Wash the precipitate produced after the reaction in step 1 with ultrapure water and centrifuge at 6000rpm, and dry the separated precipitate at a temperature of 60°C and a pressure of 0.09-0.093MPa to obtain manganese-zinc ferrite Precursor, spare; 3）将所获得的锰锌铁氧体前驱体在温度450℃、压强0.09-0.093MPa的条件下煅烧1h，即获得锰锌铁氧体粉体； 3) Calcining the obtained manganese zinc ferrite precursor at a temperature of 450°C and a pressure of 0.09-0.093 MPa for 1 hour to obtain manganese zinc ferrite powder; 二）温控磁性骨水泥的制备 2) Preparation of temperature-controlled magnetic bone cement 4）骨水泥基质的制备： 4) Preparation of bone cement matrix: 取球状聚甲基丙烯酸甲酯颗粒粉剂，经筛分后，选取粒度小于200目的球状聚甲基丙烯酸甲酯颗粒粉剂，然后在其中加入过氧化苯酰，混合均匀制得固相骨水泥基质，备用； Take spherical polymethyl methacrylate granule powder, after sieving, select spherical polymethyl methacrylate granule powder with particle size less than 200 mesh, then add benzoyl peroxide therein, and mix uniformly to obtain solid-phase bone cement matrix, spare; 所述的球状聚甲基丙烯酸甲酯的平均分子量为270kDa； The average molecular weight of described spherical polymethyl methacrylate is 270kDa; 所述的过氧化苯酰的加入量为固相骨水泥基质总重量的4 %； The addition of described benzoyl peroxide is 4% of solid-phase bone cement matrix gross weight; 另取甲基丙烯酸甲酯单体，在其中加入二甲基巯基丙酸混合均匀后制得液相骨水泥基质； Separately take methyl methacrylate monomer, add dimethyl mercaptopropionic acid to it and mix evenly to prepare liquid phase bone cement matrix; 所述的二甲基巯基丙酸的加入量为液相骨水泥基质总重量的2 %； The addition of described dimethylmercaptopropionic acid is 2% of liquid phase bone cement matrix gross weight; 5）取步骤3中制得的锰锌铁氧体粉体加入到步骤4中的骨水泥固相基质中混合均匀，制得骨水泥固相混合料；然后按照重量比为1:1的比例在骨水泥固相混合料中加入步骤4中的骨水泥液相基质，然后使用不锈钢刀调和3min即制得产品； 5) Take the manganese zinc ferrite powder prepared in step 3 and add it to the bone cement solid phase matrix in step 4 and mix evenly to obtain a bone cement solid phase mixture; then according to the ratio of 1:1 by weight Add the bone cement liquid phase matrix in step 4 to the bone cement solid phase mixture, and then use a stainless steel knife to adjust for 3 minutes to obtain the product; 其中，锰锌铁氧体粉体的加入量为最终产品总重量的40%-60%。 Wherein, the addition amount of manganese zinc ferrite powder is 40%-60% of the total weight of the final product.
CN 201210000742 2012-01-04 2012-01-04 Temperature control magnetic bone cement and preparation method thereof Expired - Fee Related CN102557527B (en)

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CN104591293A (en) * 2014-12-24 2015-05-06 合肥协知行信息系统工程有限公司 Preparation method of manganese zinc ferrite nanoparticles
CN106267330A (en) * 2016-08-29 2017-01-04 首都师范大学 A kind of bone cement with the high yield thermal efficiency
CN108129048B (en) * 2018-02-09 2020-06-23 河南科技大学 A kind of temperature-controlled magnetocaloric bone cement that can be heated rapidly and preparation method thereof
CN110251724A (en) * 2019-06-28 2019-09-20 重庆医科大学附属第二医院 A kind of doxorubicin-loaded magnetic PMMA bone cement and its preparation method and use
CN110776266B (en) * 2019-11-07 2021-10-08 郑州大学 A kind of preparation method of building material with electromagnetic wave absorption function
CN114053477B (en) * 2020-08-03 2023-06-06 首都医科大学附属北京朝阳医院 A kind of anti-myeloma nano bone cement and its preparation method and application
CN114404655B (en) * 2022-01-28 2022-12-20 洛阳市中医院 A kind of porous support with photothermal effect and preparation method thereof

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