CN107217073B - A kind of nano Pd particle-ZnO1-x@PEG@DOX gene transfer material and its preparation method and application - Google Patents

A kind of nano Pd particle-ZnO1-x@PEG@DOX gene transfer material and its preparation method and application Download PDF

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CN107217073B
CN107217073B CN201710209179.5A CN201710209179A CN107217073B CN 107217073 B CN107217073 B CN 107217073B CN 201710209179 A CN201710209179 A CN 201710209179A CN 107217073 B CN107217073 B CN 107217073B
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王深明
林颖
张德元
周鸿雁
邵楠
叶润仪
张展强
史雅微
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First Affiliated Hospital of Sun Yat Sen University
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Abstract

The present invention relates to gene transfer material technical fields, and in particular to a kind of nano Pd particle-ZnO1‑x@PEG@DOX gene transfer material and its preparation method and application.A kind of nano Pd particle-ZnO1‑xThe preparation method of@PEG@DOX gene transfer material, comprising: step 1 prepares ZnO1‑x;Step 2 prepares Pd-ZnO1‑x;Step 3 prepares Pd-ZnO1‑x@PEG;Step 4 prepares Pd-ZnO1-x@PEG@DOX, obtains nano Pd particle-ZnO1‑x@PEG@DOX gene transfer material.The nanometer gene transfer material is a kind of nanometer spherical material that average diameter is 200nm or so, when for transfecting, has the advantages that transfection efficiency is high, cell compatibility is good, cells survival rate is high;In human smooth muscle cell, the transfection efficiency of the gene transfer material reaches 55% or so.

Description

A kind of nano Pd particle-ZnO1-x@PEG@DOX gene transfer material and preparation method thereof and Using
Technical field
The present invention relates to gene transfer material technical fields, and in particular to a kind of nano Pd particle-ZnO1-x@PEG@DOX gene is led Enter material and its preparation method and application.
Background technique
With the completion that Human Genome Sequencing measures, we take the understanding of human diseases pathogenesis at the genetic level Obtained breakthrough progress.Current study show that there are many generation of disease and development are closely related with gene.If can sieve It finds and disease specifically relevant genetic fragment or gene mutation, so that it may targetedly carry out at the genetic level special Treatment, such as by importing associated deletion gene or cryptiogene, to enhance associated deletion function or silencing Disease-causing gene, thus Achieve the purpose that thoroughly to treat.Target gene is safely and effectively imported in organism be the key that in this current research field with Difficult point.
Gene delivery system or method can be divided into two classes: the first kind is virus type Gene delivery system, is with reverse transcription Virus, adenovirus, adeno-associated virus are carrier;Second class is non-virus type method of gene introduction, as microinjection, particle gun, Coprecipitation of calcium phosphate, cationic-liposome method and emerging nanometer gene transfer material is utilized to carry out gene transfection.
There are many serious deficiencies for virus type Gene delivery system or method, such as activation original is possible to when virus transfection Oncogene.Therefore, non-viral-based gene introduction method is current research hotspot, still, non-viral-based gene described above The equal Shortcomings of introduction method: microinjection can only once handle a cell, and transfection efficiency is very low;Particle gun penetrates Power is extremely limited;The transfection efficiency of calcium phosphate precipitation is influenced by many factors such as temperature, concentration, operating environments, transfection knot Fruit is very unstable;Although cationic-liposome method shows good transfection efficiency, but cationic-liposome makes because of toxicity height The application for obtaining cationic-liposome method is restricted;Nanometer gene transfer material in the prior art there are high production cost, Standby raw material processed is not easy to obtain, is difficult to the shortcomings that popularizing application.
Summary of the invention
It is an object of the present invention in view of the deficiencies of the prior art, provide a kind of nano Pd particle-ZnO1-x@PEG@DOX base Because importing the preparation method of material.
The second object of the present invention is in view of the deficiencies of the prior art, to provide a kind of nano Pd particle-ZnO1-x@PEG@DOX base Because importing material.
The third object of the present invention is in view of the deficiencies of the prior art, to provide a kind of nano Pd particle-ZnO1-x@PEG@DOX base Because importing the application of material.
One of to achieve the goals above, the present invention adopts the following technical scheme:
A kind of nano Pd particle-ZnO1-xThe preparation method of@PEG@DOX gene transfer material, it the following steps are included:
Step 1 prepares ZnO1-x: zinc chloride and stannic chloride are dissolved in water, zinc powder and glass putty is then added, stirring is equal After even, ammonium chloride and potassium hydroxide is added, then stirs certain time, obtains mixture, mixture is then transferred to reaction It in kettle, is reacted under certain temperature after a certain period of time, is successively centrifuged, is washed and is dried, obtain ZnO1-x
Step 2 prepares Pd-ZnO1-x: by ZnO made from step 11-xIt is incorporated in water, sodium tetrachloropallate is then added, Mixture is obtained, ultrasonic certain time then is carried out so that sodium tetrachloropallate is adsorbed in ZnO to the mixture1-xSurface, Then the mixture after ultrasound absorption is placed under ultraviolet light and irradiates certain time so that being adsorbed in ZnO1-xThe tetrachloro palladium on surface Sour sodium reduction is Pd atom, obtains Pd-ZnO1-x
Step 3 prepares Pd-ZnO1-x@PEG: by Pd-ZnO made from PEG2000 and step 21-xIt is scattered in dehydrated alcohol In, it after mixing evenly, is reacted under certain temperature after a certain period of time, is successively centrifuged, is washed and is dried, obtain Pd- ZnO1-x@PEG;
Step 4 prepares Pd-ZnO1-x@PEG@DOX: by Pd-ZnO made from DOX and step 31-x@PEG is scattered in water In, it then stirs after a certain period of time, is successively centrifuged, is washed and is dried, obtain nano Pd particle-ZnO1-x@PEG@DOX gene Import material.
In above-mentioned technical proposal, in step 1, zinc chloride, stannic chloride, water, zinc powder, glass putty, ammonium chloride and potassium hydroxide Mass ratio is 10 ~ 15:10 ~ 15:13 ~ 17:4 ~ 9:3 ~ 8:8 ~ 12:0.1 ~ 0.3.
In above-mentioned technical proposal, in step 1, the mixing time is 20min ~ 40min;The reaction temperature is 170 DEG C ~ 190 DEG C, the reaction time is 14h ~ 16h;
In step 1, the water is distilled water.
In above-mentioned technical proposal, in step 2, the ZnO1-xMass ratio with the water is 1:1 ~ 1.5;
In step 2, the time of the ultrasound is 6h ~ 10h;The irradiation time of the ultraviolet light is 20min ~ 40min.
In above-mentioned technical proposal, in step 2, obtained Pd-ZnO1-xIn, Pd accounts for ZnO1-xMass percent be 0.8%~1.2%。
In above-mentioned technical proposal, in step 3, PEG2000, Pd-ZnO1-xWith the mass ratio of dehydrated alcohol be 50 ~ 70:4 ~ 9:1~3;
In step 3, the reaction temperature is 170 DEG C ~ 190 DEG C, and the reaction time is 22h ~ 26h.
In above-mentioned technical proposal, in step 4, DOX, Pd-ZnO1-xThe mass ratio of@PEG and water is 1 ~ 3:8 ~ 12:3 ~ 7;
In step 4, the water is distilled water;
In step 4, the mixing time is 10h ~ 14h.
In above-mentioned technical proposal, the washing in step 3 and step 4 is to wash three times.
To achieve the goals above two, the present invention adopts the following technical scheme:
A kind of nano Pd particle-ZnO1-x@PEG@DOX gene transfer material, with a kind of nano Pd particle-ZnO described above1-x@ Nano Pd particle-ZnO obtained by the preparation method of PEG@DOX gene transfer material1-x@PEG@DOX gene transfer material, it is described to receive Rice Pd-ZnO1-x@PEG@DOX gene transfer material is a kind of nanometer spherical material that average diameter is 200nm or so.
To achieve the goals above three, the present invention adopts the following technical scheme:
A kind of nano Pd particle-ZnO described above1-xNanometer obtained by the preparation method of@PEG@DOX gene transfer material Pd-ZnO1-x@PEG@DOX gene transfer material is used to make the application of anti-tumor drug.
Compared with prior art, beneficial effect is the present invention:
A kind of nano Pd particle-ZnO provided by the invention1-xIt is received obtained by the preparation method of@PEG@DOX gene transfer material Rice Pd-ZnO1-x@PEG@DOX gene transfer material is a kind of nanometer spherical material that average diameter is 200nm or so, meets and turns Dye requires, and the Pd-ZnO of the prior art1-x@PEG@DOX particle generally can only achieve micron order, and low scale is difficult to work it out. The nanometer spherical material can with green fluorescent protein plasmid gene pGFP with non-covalent fashion in conjunction with, formed inorganic nano gene lead Enter system, is transfected for gene.Wherein, amino itself can be used for gene transfection, but the transfection efficiency of amino itself by The many factors such as temperature, concentration, operating environment influence, very unstable, are to be fixed on the invention enables amino (amino in DOX) The Pd-ZnO of this functionalization1-xThe surface@PEG@DOX, in gene transfection, amino is had an effect with the amino root in DNA again, It can achieve more stable transfection efficiency, and also can reduce the activity that high concentration amino may cause simultaneously, this will be ammonia The premise further applied in vivo after base.Compared with prior art, nano Pd particle-ZnO obtained of the present invention1-x@ PEG@DOX gene transfer material has the advantage that
(1) transfection efficiency with higher, can achieve 55% or so in human smooth muscle cell;
(2) hypotoxicity, because of nano Pd particle-ZnO1-x@PEG@DOX gene transfer material has good biocompatibility, cell Survival rate is very high;
(3) nano Pd particle-ZnO1-xThe favorable dispersibility of@PEG@DOX gene transfer material, meets the requirement to transfection;
(4) preparation cost is extremely low, and amino is food additives, cheap;In addition chemicals used in the present invention, It is the common cheap reagent being easy to get;
(5) material preparation reaction is simple, easy to operate, favorable repeatability;
(6) application prospect is good, can be applied to prepare anti-tumor drug.
Detailed description of the invention
Fig. 1 is a kind of nano Pd particle-ZnO of the invention1-xThe embodiment 1 of the preparation method of@PEG@DOX gene transfer material Obtained nano Pd particle-ZnO1-xThe scanning electron microscope (SEM) photograph of@PEG@DOX gene transfer material.
Fig. 2 is nano Pd particle-ZnO of the invention1-xUnder microscope of the@PEG@DOX gene transfer material after cell transfecting Fluorogram.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.
Wherein, " the g-C that the present invention refers to3N4" refer to graphite phase carbon nitride.
Wherein, the chemical formula for the sodium tetrachloropallate that the present invention refers to is Na2PdCl4
Wherein, the PEG2000 that the present invention refers to refers to polyethylene glycol.
Wherein, the DOX that the present invention refers to refers to adriamycin (Doxorubicin), wherein contains in the chemical structure of adriamycin There is amino.
Embodiment 1.
A kind of nano Pd particle-ZnO1-xThe preparation method of@PEG@DOX gene transfer material, it the following steps are included:
Step 1 prepares ZnO1-x: zinc chloride and stannic chloride are dissolved in water, zinc powder and glass putty is then added, stirring is equal After even, ammonium chloride and potassium hydroxide is added, then stirs 30min, obtains mixture, mixture is then transferred to reaction kettle In, after reacting 15h at 180 DEG C, successively it is centrifuged, is washed and is dried, obtain ZnO1-x;In the present embodiment, zinc chloride, Stannic chloride, water, zinc powder, glass putty, ammonium chloride and potassium hydroxide mass ratio be 13.6:13:15:6.5:5.9:10.7:0.2;Its In, water is distilled water;
Step 2 prepares Pd-ZnO1-x: by ZnO made from step 11-xIt is incorporated in water, sodium tetrachloropallate is then added, Mixture is obtained, ultrasound 8h then is carried out so that sodium tetrachloropallate is adsorbed in ZnO to the mixture1-xSurface, then will Mixture after ultrasound absorption, which is placed under ultraviolet light, irradiates 30min so that being adsorbed in ZnO1-xThe tetrachloro-palladium acid sodium reduction on surface For Pd atom, Pd-ZnO is obtained1-x;In the present embodiment, ZnO1-xMass ratio with water is 1:1;It is obtained in the present embodiment Pd-ZnO1-xIn, Pd accounts for ZnO1-xMass percent be 1%.
Step 3 prepares Pd-ZnO1-x@PEG: by Pd-ZnO made from PEG2000 and step 21-xIt is scattered in dehydrated alcohol In, after mixing evenly, after being reacted for 24 hours at 180 DEG C, successively it is centrifuged, washes three times and dry, obtain Pd-ZnO1-x@ PEG;In the present embodiment, PEG2000, Pd-ZnO1-xMass ratio with dehydrated alcohol is 62.5:6.25:2;
Step 4 prepares Pd-ZnO1-x@PEG@DOX: by Pd-ZnO made from DOX and step 31-x@PEG is scattered in water In, it after then stirring 12h, is successively centrifuged, washes three times and dry, obtain nano Pd particle-ZnO1-x@PEG@DOX gene is led Enter material.In the present embodiment, DOX, Pd-ZnO1-xThe mass ratio of@PEG and water is 2:10:5;Wherein, water is distilled water.
Wherein, nano Pd particle-ZnO made from this implementation1-x@PEG@DOX gene transfer material is that a kind of average diameter is The nanometer spherical material of 200nm or so, the nano Pd particle-ZnO1-x@PEG@DOX gene transfer material can be used in making antitumor Drug.
Embodiment 2.
A kind of nano Pd particle-ZnO1-xThe preparation method of@PEG@DOX gene transfer material, it the following steps are included:
Step 1 prepares ZnO1-x: zinc chloride and stannic chloride are dissolved in water, zinc powder and glass putty is then added, stirring is equal After even, ammonium chloride and potassium hydroxide is added, then stirs 20min, obtains mixture, mixture is then transferred to reaction kettle In, after reacting 16h at 170 DEG C, successively it is centrifuged, is washed and is dried, obtain ZnO1-x;In the present embodiment, zinc chloride, Stannic chloride, water, zinc powder, glass putty, ammonium chloride and potassium hydroxide mass ratio be 10:10:13:4:3:8:0.1;Wherein, water is double Steam water;
Step 2 prepares Pd-ZnO1-x: by ZnO made from step 11-xIt is incorporated in water, sodium tetrachloropallate is then added, Mixture is obtained, ultrasound 6h then is carried out so that sodium tetrachloropallate is adsorbed in ZnO to the mixture1-xSurface, then will Mixture after ultrasound absorption, which is placed under ultraviolet light, irradiates 20min so that being adsorbed in ZnO1-xThe tetrachloro-palladium acid sodium reduction on surface For Pd atom, Pd-ZnO is obtained1-x;In the present embodiment, ZnO1-xMass ratio with water is 1:1.2;It is obtained in the present embodiment Pd-ZnO1-xIn, Pd accounts for ZnO1-xMass percent be 0.8%.
Step 3 prepares Pd-ZnO1-x@PEG: by Pd-ZnO made from PEG2000 and step 21-xIt is scattered in dehydrated alcohol In, after mixing evenly, after reacting 26h at 170 DEG C, successively it is centrifuged, washes three times and dry, obtain Pd-ZnO1-x@ PEG;In the present embodiment, PEG2000, Pd-ZnO1-xMass ratio with dehydrated alcohol is 50:4:1;
Step 4 prepares Pd-ZnO1-x@PEG@DOX: by Pd-ZnO made from DOX and step 31-x@PEG is scattered in water In, it after then stirring 10h, is successively centrifuged, washes three times and dry, obtain nano Pd particle-ZnO1-x@PEG@DOX gene is led Enter material.In the present embodiment, DOX, Pd-ZnO1-xThe mass ratio of@PEG and water is 1:8:3;Wherein, water is distilled water.
Wherein, nano Pd particle-ZnO made from this implementation1-x@PEG@DOX gene transfer material is that a kind of average diameter is The nanometer spherical material of 200nm or so, the nano Pd particle-ZnO1-x@PEG@DOX gene transfer material can be used in making antitumor Drug.
Embodiment 3.
A kind of nano Pd particle-ZnO1-xThe preparation method of@PEG@DOX gene transfer material, it the following steps are included:
Step 1 prepares ZnO1-x: zinc chloride and stannic chloride are dissolved in water, zinc powder and glass putty is then added, stirring is equal After even, ammonium chloride and potassium hydroxide is added, then stirs 40min, obtains mixture, mixture is then transferred to reaction kettle In, after reacting 14h at 190 DEG C, successively it is centrifuged, is washed and is dried, obtain ZnO1-x;In the present embodiment, zinc chloride, Stannic chloride, water, zinc powder, glass putty, ammonium chloride and potassium hydroxide mass ratio be 15:15:17:9:8:12:0.3;Wherein, water is double Steam water;
Step 2 prepares Pd-ZnO1-x: by ZnO made from step 11-xIt is incorporated in water, sodium tetrachloropallate is then added, Mixture is obtained, ultrasound 10h then is carried out so that sodium tetrachloropallate is adsorbed in ZnO to the mixture1-xSurface, then Mixture after ultrasound absorption is placed under ultraviolet light and irradiates 40min so that being adsorbed in ZnO1-xThe sodium tetrachloropallate on surface is also Originally it was Pd atom, and obtained Pd-ZnO1-x;In the present embodiment, ZnO1-xMass ratio with water is 1:1.5;It is made in the present embodiment The Pd-ZnO obtained1-xIn, Pd accounts for ZnO1-xMass percent be 1.2%.
Step 3 prepares Pd-ZnO1-x@PEG: by Pd-ZnO made from PEG2000 and step 21-xIt is scattered in dehydrated alcohol In, after mixing evenly, after reacting 22h at 190 DEG C, successively it is centrifuged, washes three times and dry, obtain Pd-ZnO1-x@ PEG;In the present embodiment, PEG2000, Pd-ZnO1-xMass ratio with dehydrated alcohol is 70:9:3;
Step 4 prepares Pd-ZnO1-x@PEG@DOX: by Pd-ZnO made from DOX and step 31-x@PEG is scattered in water In, it after then stirring 14h, is successively centrifuged, washes three times and dry, obtain nano Pd particle-ZnO1-x@PEG@DOX gene is led Enter material.In the present embodiment, DOX, Pd-ZnO1-xThe mass ratio of@PEG and water is 3:12:7;Wherein, water is distilled water.
Wherein, nano Pd particle-ZnO made from this implementation1-x@PEG@DOX gene transfer material is that a kind of average diameter is The nanometer spherical material of 200nm or so, the nano Pd particle-ZnO1-x@PEG@DOX gene transfer material can be used in making antitumor Drug.
Embodiment 4.
A kind of nano Pd particle-ZnO1-xThe preparation method of@PEG@DOX gene transfer material, it the following steps are included:
Step 1 prepares ZnO1-x: zinc chloride and stannic chloride are dissolved in water, zinc powder and glass putty is then added, stirring is equal After even, ammonium chloride and potassium hydroxide is added, then stirs 25min, obtains mixture, mixture is then transferred to reaction kettle In, after reacting 15.5h at 175 DEG C, successively it is centrifuged, is washed and is dried, obtain ZnO1-x;In the present embodiment, chlorination Zinc, stannic chloride, water, zinc powder, glass putty, ammonium chloride and potassium hydroxide mass ratio be 12:13:16:7:6:11:0.1;Wherein, water For distilled water;
Step 2 prepares Pd-ZnO1-x: by ZnO made from step 11-xIt is incorporated in water, sodium tetrachloropallate is then added, Mixture is obtained, ultrasound 7h then is carried out so that sodium tetrachloropallate is adsorbed in ZnO to the mixture1-xSurface, then will Mixture after ultrasound absorption, which is placed under ultraviolet light, irradiates 25min so that being adsorbed in ZnO1-xThe tetrachloro-palladium acid sodium reduction on surface For Pd atom, Pd-ZnO is obtained1-x;In the present embodiment, ZnO1-xMass ratio with water is 1:1.1;It is obtained in the present embodiment Pd-ZnO1-xIn, Pd accounts for ZnO1-xMass percent be 0.9%.
Step 3 prepares Pd-ZnO1-x@PEG: by Pd-ZnO made from PEG2000 and step 21-xIt is scattered in dehydrated alcohol In, after mixing evenly, after reacting 25h at 175 DEG C, successively it is centrifuged, washes three times and dry, obtain Pd-ZnO1-x@ PEG;In the present embodiment, PEG2000, Pd-ZnO1-xMass ratio with dehydrated alcohol is 55:7:1;
Step 4 prepares Pd-ZnO1-x@PEG@DOX: by Pd-ZnO made from DOX and step 31-x@PEG is scattered in water In, it after then stirring 11h, is successively centrifuged, washes three times and dry, obtain nano Pd particle-ZnO1-x@PEG@DOX gene is led Enter material.In the present embodiment, DOX, Pd-ZnO1-xThe mass ratio of@PEG and water is 1:9:4;Wherein, water is distilled water.
Wherein, nano Pd particle-ZnO made from this implementation1-x@PEG@DOX gene transfer material is that a kind of average diameter is The nanometer spherical material of 200nm or so, the nano Pd particle-ZnO1-x@PEG@DOX gene transfer material can be used in making antitumor Drug.
Embodiment 5.
A kind of nano Pd particle-ZnO1-xThe preparation method of@PEG@DOX gene transfer material, it the following steps are included:
Step 1 prepares ZnO1-x: zinc chloride and stannic chloride are dissolved in water, zinc powder and glass putty is then added, stirring is equal After even, ammonium chloride and potassium hydroxide is added, then stirs 35min, obtains mixture, mixture is then transferred to reaction kettle In, after reacting 14.5h at 185 DEG C, successively it is centrifuged, is washed and is dried, obtain ZnO1-x;In the present embodiment, chlorination Zinc, stannic chloride, water, zinc powder, glass putty, ammonium chloride and potassium hydroxide mass ratio be 14:12:16:8:4:11:0.3;Wherein, water For distilled water;
Step 2 prepares Pd-ZnO1-x: by ZnO made from step 11-xIt is incorporated in water, sodium tetrachloropallate is then added, Mixture is obtained, ultrasound 9h then is carried out so that sodium tetrachloropallate is adsorbed in ZnO to the mixture1-xSurface, then will Mixture after ultrasound absorption, which is placed under ultraviolet light, irradiates 35min so that being adsorbed in ZnO1-xThe tetrachloro-palladium acid sodium reduction on surface For Pd atom, Pd-ZnO is obtained1-x;In the present embodiment, ZnO1-xMass ratio with water is 1:1.4;It is obtained in the present embodiment Pd-ZnO1-xIn, Pd accounts for ZnO1-xMass percent be 1.1%.
Step 3 prepares Pd-ZnO1-x@PEG: by Pd-ZnO made from PEG2000 and step 21-xIt is scattered in dehydrated alcohol In, after mixing evenly, after reacting 23h at 185 DEG C, successively it is centrifuged, washes three times and dry, obtain Pd-ZnO1-x@ PEG;In the present embodiment, PEG2000, Pd-ZnO1-xMass ratio with dehydrated alcohol is 65:7:2;
Step 4 prepares Pd-ZnO1-x@PEG@DOX: by Pd-ZnO made from DOX and step 31-x@PEG is scattered in water In, it after then stirring 13h, is successively centrifuged, washes three times and dry, obtain nano Pd particle-ZnO1-x@PEG@DOX gene Import material.In the present embodiment, DOX, Pd-ZnO1-xThe mass ratio of@PEG and water is 1:11:6;Wherein, water is distilled water.
Wherein, nano Pd particle-ZnO made from this implementation1-x@PEG@DOX gene transfer material is that a kind of average diameter is The nanometer spherical material of 200nm or so, the nano Pd particle-ZnO1-x@PEG@DOX gene transfer material can be used in making antitumor Drug.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected The limitation of range is protected, although explaining in detail referring to preferred embodiment to the present invention, those skilled in the art are answered Work as understanding, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the reality of technical solution of the present invention Matter and range.

Claims (10)

1. a kind of nano Pd particle-ZnO1-xThe preparation method of@PEG@DOX gene transfer material, it is characterised in that: it includes following step It is rapid:
Step 1 prepares ZnO1-x: zinc chloride and stannic chloride are dissolved in water, zinc powder and glass putty is then added, stirs evenly Afterwards, ammonium chloride and potassium hydroxide is added, then stirs certain time, obtains mixture, mixture is then transferred to reaction kettle In, it is reacted under certain temperature after a certain period of time, is successively centrifuged, is washed and is dried, obtain ZnO1-x
Step 2 prepares Pd-ZnO1-x: by ZnO made from step 11-xIt is incorporated in water, sodium tetrachloropallate is then added, obtain Then mixture carries out ultrasonic certain time so that sodium tetrachloropallate is adsorbed in ZnO to the mixture1-xSurface, then Mixture after ultrasound absorption is placed under ultraviolet light and irradiates certain time so that being adsorbed in ZnO1-xThe sodium tetrachloropallate on surface It is reduced to Pd atom, obtains Pd-ZnO1-x
Step 3 prepares Pd-ZnO1-x@PEG: by Pd-ZnO made from PEG2000 and step 21-xIt is scattered in dehydrated alcohol, After mixing evenly, it is reacted under certain temperature after a certain period of time, is successively centrifuged, is washed and is dried, obtain Pd-ZnO1-x@ PEG;
Step 4 prepares Pd-ZnO1-x@PEG@DOX: by Pd-ZnO made from DOX and step 31-x@PEG is dispersed in water, so After stir after a certain period of time, be successively centrifuged, washed and dried, obtain nano Pd particle-ZnO1-x@PEG@DOX channel genes material Material.
2. a kind of nano Pd particle-ZnO according to claim 11-xThe preparation method of@PEG@DOX gene transfer material, it is special Sign is: in step 1, zinc chloride, stannic chloride, water, zinc powder, glass putty, ammonium chloride and potassium hydroxide mass ratio be 10~15: 10~15:13~17:4~9:3~8:8~12:0.1~0.3.
3. a kind of nano Pd particle-ZnO according to claim 11-xThe preparation method of@PEG@DOX gene transfer material, it is special Sign is: in step 1, the mixing time is 20min~40min;The reaction temperature is 170 DEG C~190 DEG C, described anti- It is 14h~16h between seasonable;
In step 1, the water is distilled water.
4. a kind of nano Pd particle-ZnO according to claim 11-xThe preparation method of@PEG@DOX gene transfer material, it is special Sign is: in step 2, the ZnO1-xMass ratio with the water is 1:1~1.5;
In step 2, the time of the ultrasound is 6h~10h;The irradiation time of the ultraviolet light is 20min~40min.
5. a kind of nano Pd particle-ZnO according to claim 11-xThe preparation method of@PEG@DOX gene transfer material, it is special Sign is: in step 2, obtained Pd-ZnO1-xIn, Pd accounts for ZnO1-xMass percent be 0.8%~1.2%.
6. a kind of nano Pd particle-ZnO according to claim 11-xThe preparation method of@PEG@DOX gene transfer material, it is special Sign is: in step 3, PEG2000, Pd-ZnO1-xMass ratio with dehydrated alcohol is 50~70:4~9:1~3;
In step 3, the reaction temperature is 170 DEG C~190 DEG C, and the reaction time is 22h~26h.
7. a kind of nano Pd particle-ZnO according to claim 11-xThe preparation method of@PEG@DOX gene transfer material, it is special Sign is: in step 4, DOX, Pd-ZnO1-xThe mass ratio of@PEG and water is 1~3:8~12:3~7;
In step 4, the water is distilled water;
In step 4, the mixing time is 10h~14h.
8. a kind of nano Pd particle-ZnO according to claim 11-xThe preparation method of@PEG@DOX gene transfer material, it is special Sign is: the washing in step 3 and step 4 is to wash three times.
9. a kind of nano Pd particle-ZnO1-x@PEG@DOX gene transfer material, it is characterised in that: any one with claim 1 to 8 A kind of nano Pd particle-ZnO described in1-xNano Pd particle-ZnO obtained by the preparation method of@PEG@DOX gene transfer material1-x@ PEG@DOX gene transfer material, the nano Pd particle-ZnO1-xIt is 200nm that@PEG@DOX gene transfer material, which is a kind of average diameter, Nanometer spherical material.
10. a kind of nano Pd particle-ZnO described in claim 1 to 8 any one1-xThe preparation side of@PEG@DOX gene transfer material Nano Pd particle-ZnO obtained by method1-x@PEG@DOX gene transfer material is used to make the application of anti-tumor drug.
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