CN103550791B - Preparation and application of water-soluble magnetic targeting carbon composite material - Google Patents
Preparation and application of water-soluble magnetic targeting carbon composite material Download PDFInfo
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- CN103550791B CN103550791B CN201310514242.8A CN201310514242A CN103550791B CN 103550791 B CN103550791 B CN 103550791B CN 201310514242 A CN201310514242 A CN 201310514242A CN 103550791 B CN103550791 B CN 103550791B
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Abstract
The invention relates to a preparation method of a water-soluble magnetic targeting carbon composite material and application of the water-soluble magnetic targeting carbon composite material in a medicine for diagnosing and treating tumor, and the water-soluble magnetic targeting carbon composite material can be used for solving the problems that the tumor curative effect is bad, the targeting is bad, and the toxic and side effect are great. The technical scheme of the water-soluble magnetic targeting carbon composite material is as follows: placing 10-20 mg of carbon material in 20 ml of mixed solution composed of ethylene glycol and diolacetal at a volume ratio of 1:19, stirring, ultrasonically dispersing uniformly, orderly adding 0.15-0.3 g of sodium acetate and 0.27-0.54 g of gadolinium chloride while stirring, sufficiently dissolving under ultrasonic, transferring to a reaction kettle, reacting for 10 hours at 200 DEG C, after the reaction, leaching and rinsing for 3-5 times by orderly using absolute ethyl alcohol and ultrapure water, obtaining a filter cake, performing vacuum drying for 24-56 hours at 20-60 DEG C to obtain the water-soluble magnetic targeting carbon composite material. The water-soluble magnetic targeting carbon composite material is good in biological compatibility, high in magnetic targeting, and small in side effect, can be effectively used for magnetic resonance contrast agents and medicines for diagnosing and treating tumors, and has great clinical significance.
Description
Technical field
The present invention relates to drug world, particularly a kind of preparation of water-soluble magnetic targeting carbon composite and application thereof.
Background technology
Carbon nanomaterial is more and more extensive as the application on pharmaceutical carrier in recent years.In carbon nanomaterial, the carbon nanomaterial comprising fullerene, CNT and graphene oxide is one of Disciplinary Frontiers of international scientific in recent years always.In recent years, fullerene is quite noticeable in the research of biomedicine field, and research finds that fullerene has multiple special biological effect: (1) can suppress the activity of multiple enzyme, comprises hiv protease and reverse transcriptase; (2) cytotoxicity is demonstrated to tumor cell; (3) there is the effect of neuroprotective; (4) also there is the effect producing oxygen-derived free radicals, cutting DNA under visible light illumination.As a kind of excellent photosensitizer, fullerene shows that it can produce active oxygen when radiation of visible light, active oxygen comprises singlet oxygen, superoxide anion etc., obvious cytotoxicity can be shown, DNA in such as cell lysis, the mitosis of T suppression cell and growth, the activity of all right T suppression cell proteolytic enzyme, fullerene may be used for the treatment of tumor as photosensitizer.
NMR (Nuclear Magnetic Resonance)-imaging (Nuclear Magnetic Resonance Imaging, NMRI) technology is a kind of new Image Examination risen over nearly 20 years. in clinical diagnosis, utilize NMR (Nuclear Magnetic Resonance) imaging reinforcing agent, sweep time can be shortened and obtain image more clearly.As medicinal application in the MRI contrast agent of human body and nuclear-magnetism probe except should meet medicine basic demand and good water solubility and except self having enough stability, also should meet following characteristic: (1) high relaxation rate; (2) targeting, reduces the non-specific adsorption at non-lesions position; (3) toxic and side effects is low; (4) there is suitable retention time in vivo, and be easy to get rid of in body.
The general designation of lanthanide series (lanthanide element) to be periodic system of elements III B race Atom ordinal number be 15 kinds of chemical elements of 57 ~ 71.Because lanthanide series is all metal, so also known as lanthanide series metal.Comprise lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutecium.Lanthanide series metal has silvery white or Lycoperdon polymorphum Vitt gloss, and quality is softer, has ductility, and activity is very strong.Lanthanide series metal 4f electronic structure determines the magnetic property of this metal and compound thereof.The magnetic of material is produced by unpaired electron, and the more, its magnetic moment and susceptibility are larger for outer unpaired electron number.Except La (4f
0) and Lu (4f
14) outside be all paramagnetic ion, may be used for NMR (Nuclear Magnetic Resonance) imaging.For gadolinium (Gd): Gd(III) its relaxation rate of carbon nanomaterial significantly improve, load Gd(III) afterwards its t1 shorten to 2701ms by original 20147ms.For obtaining the magnetic resonance contrast agent of high relaxation rate, utilize nano-carrier technology, by nano-carrier surface coupling with the macromolecule of a large amount of amino group, more Gd(III are provided) load site, restriction Gd(III) rotation, strengthen Gd(III) rigidity of derivant improves relaxivity.
Material with carbon element is combined with magnetic material and forms water-soluble magnetic targeting carbon composite by the present invention, not only there is magnetic targeted, under magnetic field, medicine long time high concentration is made to be gathered in tumor locus, strengthen drug effect, reduce side effect, but also remain the photosensitive of material with carbon element self, temperature-sensitive etc. characteristic, in illumination, under the conditions such as radio frequency, active oxygen can be produced, kill tumor cell, strengthen the curative effect of medicine, this water-soluble magnetic targeting carbon composite can be used as pharmaceutical carrier, magnetic resonance contrast agent is applied to diagnoses and treatment tumor, overcome at present that targeting is poor clinically, the problems such as side effect is large, there is great potential applicability in clinical practice.
Summary of the invention
For above-mentioned situation, overcome the defect of prior art, the object of the present invention is just to provide a kind of preparation method of water-soluble magnetic targeting carbon composite, effectively can solve the problems such as treatment tumor-targeting is poor, toxic and side effects is large.
The technical scheme that the present invention solves is, material with carbon element 10-20mg is placed in 20ml by ethylene glycol and the two acetals mixed solvent that forms of 1:19 by volume, stir, ultrasonicly it is made to be uniformly dispersed, under agitation, add sodium acetate 0.15-0.3g and Gadolinium trichloride 0.27-0.54g successively, after ultrasonic abundant dissolving, be transferred in reactor, 200 DEG C of reaction 10h, after reaction terminates, add dehydrated alcohol 50-100ml, ultrasonic, with 0.22um microporous filter membrane sucking filtration, and with 20ml dehydrated alcohol rinse filter cake, after filter cake is proceeded in beaker, add dehydrated alcohol 50-100ml, ultrasonic, use 0.22um microporous filter membrane sucking filtration again, and with 20ml dehydrated alcohol rinse filter cake, repeat operation 3 times, again filter cake is proceeded in beaker, add ultra-pure water 50-100ml, ultrasonic, with 0.45um microporous filter membrane sucking filtration, and with 20ml ultra-pure water rinse filter cake, repeat operation 5 times, the filter cake obtained is at 20-60 DEG C, vacuum drying 24-56h, obtains gadolinium load-type composite material derivant, i.e. water-soluble magnetic targeting carbon composite, described material with carbon element is the one of fullerene and derivant, CNT and derivant thereof, graphene oxide and derivant thereof.
Synthesis technique of the present invention is simple and convenient, has the advantages such as good biocompatibility, magnetic targeted, hypotoxicity, and being effective to diagnosis, treatment tumor as magnetic resonance (imaging) contrast agent medicine, is that on diagnoses and treatment tumour medicine innovates greatly.
Detailed description of the invention
Below in conjunction with embodiment, the specific embodiment of the present invention is described in further detail.
Embodiment 1
Preparation method of the present invention is in concrete enforcement, and (1), by the method for number of patent application 201210406707.3, carries out amination modification to fullerene, obtains the fullerene that amination is modified, (2) the fullerene 20mg that amination is modified is placed in 20ml by ethylene glycol and the two acetals mixed solvent that forms of 1:19 by volume, stir, ultrasonicly it is made to be uniformly dispersed, under agitation, add sodium acetate 0.3g and Gadolinium trichloride 0.54g successively, after ultrasonic abundant dissolving, be transferred in reactor, 200 DEG C of reaction 10h, after reaction terminates, add dehydrated alcohol 100ml, ultrasonic, with 0.22um microporous filter membrane sucking filtration, and with 20ml dehydrated alcohol rinse filter cake, after filter cake is proceeded in beaker, add dehydrated alcohol 100ml, ultrasonic, use 0.22um microporous filter membrane sucking filtration again, and with 20ml dehydrated alcohol rinse filter cake, repeat operation 3 times, again filter cake is proceeded in beaker, add ultra-pure water 100ml, ultrasonic, with 0.45um microporous filter membrane sucking filtration, and with 20ml ultra-pure water rinse filter cake, repeat operation 5 times, the filter cake obtained is at 60 DEG C, vacuum drying 56h, obtains gadolinium load fullerene derivate, i.e. water-soluble magnetic targeting carbon composite.
Embodiment 2
Preparation method of the present invention is in concrete enforcement, CNT 20mg is placed in 20ml by ethylene glycol and the two acetals mixed solvent that forms of 1:19 by volume, stir, ultrasonicly it is made to be uniformly dispersed, under agitation, add sodium acetate 0.3g and Gadolinium trichloride 0.54g successively, after ultrasonic abundant dissolving, be transferred in reactor, 200 DEG C of reaction 10h, after reaction terminates, add dehydrated alcohol 100ml, ultrasonic, with 0.22um microporous filter membrane sucking filtration, and with 20ml dehydrated alcohol rinse filter cake, after filter cake is proceeded in beaker, add dehydrated alcohol 100ml, ultrasonic, use 0.22um microporous filter membrane sucking filtration again, and with 20ml dehydrated alcohol rinse filter cake, repeat operation 3 times, again filter cake is proceeded in beaker, add ultra-pure water 100ml, ultrasonic, with 0.45um microporous filter membrane sucking filtration, and with 20ml ultra-pure water rinse filter cake, repeat operation 5 times, the filter cake obtained is at 60 DEG C, vacuum drying 48h, obtains gadolinium load CNT, i.e. water-soluble magnetic targeting carbon compound material.
Embodiment 3
Preparation method of the present invention is in concrete enforcement, graphene oxide 10mg is placed in 20ml by ethylene glycol and the two acetals mixed solvent that forms of 1:19 by volume, stir, ultrasonicly it is made to be uniformly dispersed, under agitation, add sodium acetate 0.15g and Gadolinium trichloride 0.27g successively, after ultrasonic abundant dissolving, be transferred in reactor, 200 DEG C of reaction 10h, after reaction terminates, add dehydrated alcohol 50, ultrasonic, with 0.22um microporous filter membrane sucking filtration, and with 20ml dehydrated alcohol rinse filter cake, after filter cake is proceeded in beaker, add dehydrated alcohol 50ml, ultrasonic, use 0.22um microporous filter membrane sucking filtration again, and with 20ml dehydrated alcohol rinse filter cake, repeat operation 3 times, again filter cake is proceeded in beaker, add ultra-pure water 50, ultrasonic, with 0.45um microporous filter membrane sucking filtration, and with 20ml ultra-pure water rinse filter cake, repeat operation 5 times, the filter cake obtained is at 50 DEG C, vacuum drying 32h, obtains gadolinium load graphene oxide, i.e. water-soluble magnetic targeting carbon composite.
The application of water-soluble magnetic targeting carbon composite of the present invention in diagnoses and treatment tumor, correlation test data is as follows:
12 mice completely randoms of inoculation mouse breast cancer tumour are divided into experimental group and matched group, and 6 experiment mices inject the water-soluble magnetic targeting gadolinium load graphene oxide solution 200ul of 2mg/ml through tail vein.And 6 control group mice do not deal with.The anesthesia of mice is 3% pentobarbital sodium 0.04ml, lumbar injection, and carries out MR imaging after (i.e. 0h) and injection 24h before injection water dissolubility magnetic targeted gadolinium load graphene oxide and derivative solution thereof.At the T2WI image rendering induction zone ROI of the same size of 0h and 24h experimental group and control group mice tumor region, measure tumor entity fraction of signal strength (SI
t), get its meansigma methods, measured area is not less than 6mm
2.Add up Soft Roll with spss19.0, measurement data compound normal distributes, and be expressed as x ± s, what be not inconsistent represents with median (M).During 0h and 24h time experimental group and matched group between tumor entity fraction of signal strength (SI
t) compare with two independent samples t test.P<0.05 is that difference has statistical significance, and p<0.01 thinks that difference has height statistical significance.
After the same method, water-soluble magnetic targeting gadolinium load CNT, gadolinium load fullerene are measured, experiment proves: water-soluble magnetic targeting gadolinium load graphene oxide of the present invention, gadolinium load CNT, gadolinium load fullerene can as magnetic resonance imaging contrast, diagnosing tumour, detection of drugs.
Water-soluble magnetic targeting carbon composite of the present invention is as the application of magnetic target medicine transport vehicle in diagnoses and treatment tumor, and detailed process is following step:
(1) by water-soluble magnetic targeting gadolinium load graphene oxide and antitumor drug by ultrasonic, stir, visit super or rotary evaporation and combine.
(2) the water-soluble magnetic targeting gadolinium load graphene oxide of drug loading carried out antitumor cell and suppress in-vivo tumour evaluation.
Described antitumor drug is: insoluble anti-tumor medicament, water-soluble anti-tumor medicine and nucleic acid drug, such as: one or more in Docetaxel, paclitaxel, amycin, cisplatin, carboplatin, daunorubicin, few adopted antinucleus thuja acid, RNA interfering and enzyme drug.
Described antitumor cell is: organ surface or the inner various solid tumors occurred, pulmonary carcinoma, nasopharyngeal carcinoma, esophageal carcinoma, gastric cancer, hepatocarcinoma, colorectal cancer, breast carcinoma, ovarian cancer, bladder cancer, leukemia, cancer of pancreas, cervical cancer, laryngeal carcinoma, thyroid carcinoma, carcinoma of tongue, cerebroma (intracranial tumor), intestinal tumor, carcinoma of gallbladder, cancer of biliary duct, renal carcinoma, carcinoma of prostate, carcinoma of penis, tumor of testis, carcinoma of endometrium, choriocarcinoma, For Primary Vaginal Carcinoma, Vulvar, Hodgkin, non-Hodgkin lymphoma, skin carcinoma, one in malignant melanoma.
Described tumor D is: organ surface or the inner various solid tumors occurred, pulmonary carcinoma, nasopharyngeal carcinoma, esophageal carcinoma, gastric cancer, hepatocarcinoma, colorectal cancer, breast carcinoma, ovarian cancer, bladder cancer, leukemia, cancer of pancreas, cervical cancer, laryngeal carcinoma, thyroid carcinoma, carcinoma of tongue, cerebroma (intracranial tumor), intestinal tumor, carcinoma of gallbladder, cancer of biliary duct, renal carcinoma, carcinoma of prostate, carcinoma of penis, tumor of testis, carcinoma of endometrium, choriocarcinoma, For Primary Vaginal Carcinoma, Vulvar, Hodgkin, non-Hodgkin lymphoma, skin carcinoma, the one in malignant melanoma.
Experiment proves, water-soluble magnetic targeting carbon composite of the present invention, as drug delivery carrier, under the effect of externally-applied magnetic field, can combine in tumor region by targeting poly, and compared with normal cell, it can long-term high concentration be retained in tumor region.
Water-soluble magnetic targeting carbon composite of the present invention can make arbitrary medicament form of pharmaceutical preparation as drug delivery carrier, such as: injection, aseptic powder needle for injection, dispersant, patch, gel, implant etc.; And the additive of various preparation can be added, such as: normal saline, glucose, buffer solution and antiseptic etc. are so that be prepared into the dosage form of needs, and administering mode can be: intravenous injection, intramuscular injection, intratumor injection and subcutaneous injection, transdermal administration, et al. Ke mode etc.
Water-soluble magnetic targeting carbon composite of the present invention is divided in vitro and in vivo two parts as the application of heat sensitizer diagnoses and treatment tumor, and specific experiment content is as follows:
(1) illumination jetting dissolubility magnetic targeted gadolinium load graphene oxide anti-tumor activity is in vitro used
By PC3 prostate gland cancer cell (being provided by Shanghai cell bank) as cancerous cell to be investigated, cultivated by PC3 cancerous cell and containing hyclone (FBS) 10%, in the RPMI1640 culture medium of mycillin mixed liquor 1%, incubator condition is 37 DEG C, 5%CO
2, within every 2 ~ 3 days, go down to posterity once.Collect logarithmic (log) phase cell, adjustment concentration of cell suspension, the 96 every holes of orifice plate add 200ul, and bed board makes cell to be measured adjust density to 6 × 10
3individual/hole, (the aseptic PBS of edge hole fills).Be placed in 5%CO
2, hatch 24h for 37 DEG C, be paved with (96 hole flat underside) at the bottom of hole to cell monolayer, add the water-soluble magnetic targeting gadolinium load graphene oxide solution in the embodiment 1 of Concentraton gradient (12.5,25,50,100 μ g/ml).Light group is placed on 2min in 808nm near-infrared 2W, and in maintenance During Illumination, temperature is at 37 DEG C, and illumination terminates rear aluminium-foil paper parcel cell plates as CO
2hatch 24h in incubator, for not light group, then direct aluminium-foil paper parcel cell plates are as CO
2hatch 24h in incubator, stop cultivating, sucking-off pastille culture medium, every hole 150ulPBS washes 2 times, adds the 10%TCA200ul of pre-cooling, places 1h for 4 DEG C.Outwell fixative, every hole deionized water washes 5 times, dries, air drying.Every hole adds the SRB solution of 100ul, leaves standstill and places 10min, be positioned at protein bound SRB 1% acetic acid and wash 5 times, air drying.In conjunction with SRB 150ul10mmol/L non-buffered liquid Tris alkali dissolution.The OD value in every hole is measured at 808nm place.The computing formula of survival rate: survival rate=experimental group OD value/matched group OD value, wherein experimental group and matched group are the value after deducting blank group.
Experiment prove, when use up irradiate 2min, water-soluble target tropism carbon composite of the present invention add the increment that directly affects PC3 cell.
(2) when illumination is penetrated, the mensuration of water-soluble magnetic targeting gadolinium load graphene oxide anti-tumor in vivo activity of the present invention:
Get mouse S180 ascites sarcoma cell, with injection normal saline with after volume ratio 3:1 dilution, every mice, in lumbar injection 0.3ml, after mice feeds 7 days, extracts mouse S180 ascites sarcoma cell, becomes concentration for 2 × 10 after counting with injection normal saline dilution
6the cell suspension in individual/hole, subcutaneous vaccination and mice right fore top.After mouse inoculation tumor 7d, get wherein 24 gross tumor volume>=100mm
3kunming mice, is divided into 4 groups at random, often organizes 6.Specifically be grouped as follows: (1) matched group (NS group): normal saline; (2) normal saline laser group; (3) water-soluble target tropism gadolinium load graphene oxide group; (4) water-soluble target tropism gadolinium load graphene oxide laser group.4 groups all adopt intravenous administration approach, and the light source that wherein light group uses is 808nm near-infrared light source, and power is 2W, and after administration 3h, laser irradiates tumor locus, and the once irradiating time is 2min.Every 2d is administered once, the water-soluble target tropism gadolinium load graphene oxide 100 μ l of per injection normal saline or 2mg/ml, altogether administration 7 times.In whole experimentation, every day observes the animation of mice, within every two days, claims its body weight and uses the major diameter (A) of vernier caliper measurement murine sarcoma and minor axis (B), by formula
calculate gross tumor volume.
Experiment proves, water-soluble magnetic targeting carbon composite of the present invention when irradiating in conjunction with laser, the increase of mouse tumor volume obtains obvious suppression.
When water-soluble magnetic targeting carbon composite of the present invention carries out advanced tumors in temperature-sensitive treatment body as heat sensitizer, 808nm laser the degree of depth can penetrate organism, may be used for treating tumor.
Water-soluble magnetic targeting carbon composite of the present invention can make arbitrary pharmaceutical preparation as heat sensitizer, such as: injection, aseptic powder needle for injection, dispersant, patch, gel, implant etc., and the additive of various preparation can be added, such as: normal saline, glucose, buffer solution and antiseptic etc. are prepared into the dosage form of needs, administering mode can be: intravenous injection, intramuscular injection, intratumor injection and subcutaneous injection, transdermal administration, et al. Ke etc.
Experimental data shows:
(1) water-soluble magnetic targeting carbon composite of the present invention is as the carrier of medicine in diagnoses and treatment tumor, has magnetic targeted, under magnetic field, makes medicine long time high concentration be gathered in tumor locus, strengthens drug effect, reduces side effect.
(2) water-soluble magnetic targeting carbon composite of the present invention, has NMR (Nuclear Magnetic Resonance) imaging, over the course for the treatment of, utilizes NMR (Nuclear Magnetic Resonance) imaging diagnosis of technique tumor, monitoring medicine.
(3) water-soluble magnetic targeting carbon composite of the present invention, can not itself destroying material with carbon element, retains the characteristic of material with carbon element self, as heliosensitivity, thermal sensitivity, under the condition such as illumination, radio frequency, active oxygen can be produced, kill tumor cell, strengthen the curative effect of medicine.Be the innovation in diagnosis, tumor, be conducive to the treatment of tumor patient, rehabilitation, have actual clinical meaning, economic and social benefit is huge.
Claims (4)
1. the preparation method of a water-soluble magnetic targeting carbon composite, it is characterized in that, material with carbon element 10-20mg is placed in 20ml by ethylene glycol and the two acetals mixed solvent that forms of 1:19 by volume, stir, ultrasonicly it is made to be uniformly dispersed, under agitation, add sodium acetate 0.15-0.3g and Gadolinium trichloride 0.27-0.54g successively, after ultrasonic abundant dissolving, be transferred in reactor, 200 DEG C of reaction 10h, after reaction terminates, add dehydrated alcohol 50-100ml, ultrasonic, with 0.22 μm of microporous filter membrane sucking filtration, and with 20ml dehydrated alcohol rinse filter cake, after filter cake is proceeded in beaker, add dehydrated alcohol 50-100ml, ultrasonic, filter cake is obtained again with 0.22 μm of microporous filter membrane sucking filtration, with 20ml dehydrated alcohol rinse filter cake, repeat operation 3 times, again filter cake is proceeded in beaker, add ultra-pure water 50-100ml, ultrasonic, with 0.45 μm of microporous filter membrane sucking filtration, and with 20ml ultra-pure water rinse filter cake, repeat operation 5 times, the filter cake obtained is at 20-60 DEG C, vacuum drying 24-56h, obtains gadolinium load-type composite material derivant, i.e. water-soluble magnetic targeting carbon composite, described material with carbon element is the one of fullerene, CNT or graphene oxide.
2. the preparation method of water-soluble magnetic targeting carbon composite according to claim 1, it is characterized in that, CNT 20mg is placed in 20ml by ethylene glycol and the two acetals mixed solvent that forms of 1:19 by volume, stir, ultrasonicly it is made to be uniformly dispersed, under agitation, add sodium acetate 0.3g and Gadolinium trichloride 0.54g successively, after ultrasonic abundant dissolving, be transferred in reactor, 200 DEG C of reaction 10h, after reaction terminates, add dehydrated alcohol 100ml, ultrasonic, with 0.22 μm of microporous filter membrane sucking filtration, and with 20ml dehydrated alcohol rinse filter cake, after filter cake is proceeded in beaker, add dehydrated alcohol 100ml, ultrasonic, use 0.22 μm of microporous filter membrane sucking filtration again, and with 20ml dehydrated alcohol rinse filter cake, repeat operation 3 times, again filter cake is proceeded in beaker, add ultra-pure water 100ml, ultrasonic, with 0.45 μm of microporous filter membrane sucking filtration, and with 20ml ultra-pure water rinse filter cake, repeat operation 5 times, the filter cake obtained is at 60 DEG C, vacuum drying 48h, obtains gadolinium load CNT, i.e. water-soluble magnetic targeting carbon compound material.
3. the preparation method of water-soluble magnetic targeting carbon composite according to claim 1, it is characterized in that, graphene oxide 10mg is placed in 20ml by ethylene glycol and the two acetals mixed solvent that forms of 1:19 by volume, stir, ultrasonicly it is made to be uniformly dispersed, under agitation, add sodium acetate 0.15g and Gadolinium trichloride 0.27g successively, after ultrasonic abundant dissolving, be transferred in reactor, 200 DEG C of reaction 10h, after reaction terminates, add dehydrated alcohol 50, ultrasonic, with 0.22 μm of microporous filter membrane sucking filtration, and with 20ml dehydrated alcohol rinse filter cake, after filter cake is proceeded in beaker, add dehydrated alcohol 50ml, ultrasonic, use 0.22 μm of microporous filter membrane sucking filtration again, and with 20ml dehydrated alcohol rinse filter cake, repeat operation 3 times, again filter cake is proceeded in beaker, add ultra-pure water 50ml, ultrasonic, with 0.45 μm of microporous filter membrane sucking filtration, and with 20ml ultra-pure water rinse filter cake, repeat operation 5 times, the filter cake obtained is at 50 DEG C, vacuum drying 32h, obtains gadolinium load graphene oxide, i.e. water-soluble magnetic targeting carbon composite.
4. the water-soluble magnetic targeting carbon composite that prepared by claim 1 or any one of 2-3 method is preparing the application in diagnoses and treatment tumor magnetic resonance radiography agent medicine.
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