CN105251012B - Nanogold coats layered double-hydroxide composite and its preparation and application - Google Patents
Nanogold coats layered double-hydroxide composite and its preparation and application Download PDFInfo
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Abstract
The present invention relates to nanogold cladding layered double-hydroxide composite and its preparation and application, the composite is core-shell structure, outside is enclosed with the double-hydroxide particle of nano Au particle, the average grain diameter of nano Au particle is less than 5nm, the particle diameter of double-hydroxide particle is 20 200nm, can apply to medicine delivery.Compared with prior art, the composite that the present invention is prepared has pH sensitiveness, high drug load, internal field cyclicity, surface potential positive and negative can be modified, surface can link aglucon, antibody, amination, carboxylated, aldehyde radical, for pharmaceutical carrier, reach the double action of targeting and sustained release in vivo, improve circulation time, drug availability, target-oriented drug inside medicine.
Description
Technical field
The present invention relates to a kind of medicine-carried system, more particularly, to nanogold coat layered double-hydroxide composite and its
Prepare and apply.
Background technology
Layered double hydroxide (LDH) is a kind of novel nano inorganic functional material for having layer structure, brilliant in LDH
In body structure, due to being influenceed by the minimum effect of lattice energy and its lattice orientation effect so that metal ion is on laminate with one
Determine mode to be uniformly distributed, i.e., on laminate in each micro-structure unit, its chemical composition and structure is constant, and is located at interlayer
Anion due to being limited by the attracting of laminate electric charge, the repulsion between interlayer ion, inner layer space, distribution is also very uniform.
Chinese patent CN104274838 A disclose kind of dexamethasone sodium phosphate/layered double-hydroxide in treating asthma
Application of aspect and preparation method thereof.It is big for conventional sugar cortex agent dexamethasone phosphoric acid sodium toxicity, the shortcomings that targeting difference,
Dexamethasone sodium phosphate is carried using layered double-hydroxide, for improving the therapeutic effect of dexamethasone sodium phosphate,
Reduce the toxic side effect of dexamethasone sodium phosphate.But because the patent does not have composite nano-gold, the targeting of medicine is relatively
It is low to cause drug availability poor, so as to cause curative effect relatively weak.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of nanogold clad
Shape double-hydroxide composite and its preparation and application, for pharmaceutical carrier, reach targeting and the dual work being sustained in vivo
With circulation time, drug availability, target-oriented drug inside raising medicine.
The purpose of the present invention can be achieved through the following technical solutions：
Nanogold coats layered double-hydroxide composite, is core-shell structure, outside is enclosed with nano Au particle
Double-hydroxide particle,
The average grain diameter of described nano Au particle is less than 5nm, and the particle diameter of described double-hydroxide particle is 20-
200nm。
The content of nanogold is 10 in composite-5mol/L。
Contain bivalent metal ion and trivalent metal ion in double-hydroxide, interlayer contains anion.
Described bivalent metal ion is Mg2+、Mn2+、Fe2+、Co2+、Ni2+、Cu2+Or Zn2+Middle one or two, trivalent gold
Category ion is Al3+、Cr3+、Mn3+、Fe3+、Co3+Or Ni3+Middle one or two, the anion that interlayer contains are OH-、CO3 2-、
SO4 2-、Cl-Or NO3 -One or both of.
Nanogold coats the preparation method of layered double-hydroxide composite, using following steps：
(1) preparation of nano layered double hydroxides
A, prepare salt containing bivalent metal ion and trivalent metal ion salts solution, bivalent metal ion salt and trivalent metal from
Mol ratio between alite is 1：3；
B, NaOH solution is configured and in N2The lower 60 DEG C of stirrings 10min of atmosphere；
C, step a solution is added drop-wise in step b solution, N2Lower 60 DEG C of atmosphere continues to stir 3h；
D, sample taking-up will be obtained after reaction, is cleaned and centrifuged 3 times repeatedly using distilled water after centrifugation, then be placed in hydro-thermal
Kettle, 100 DEG C of reaction 16h；
E, the sample centrifugal treating that will be obtained, supernatant is removed, is placed in vacuum drying chamber 50 DEG C and is completely dried 48 hours
After take out, be placed in grind into powder in mortar, obtain nano layered double hydroxides；
(2) preparation of nanogold
A, four n-octyl ammonium bromides, lauryl amine, gold chloride are dissolved in toluene, are at room temperature added to sodium borohydride acutely
In the above-mentioned mixed solution of stirring, four n-octyl ammonium bromides, lauryl amine, gold chloride, the mol ratio of sodium borohydride are 0.2-0.3：
0.5-0.7：0.4-0.6：1-3, progress high speed centrifugation obtains oil-soluble nanogold after mixing 2h.
B, gained nanogold is dissolved in chloroform, with molecular weight 2000, the functional polyethylene glycol HS- containing sulfydryl and carboxyl
PEG-COOH modified nano golds surface, reacts 24h at room temperature, obtains stable 5nm nanogold systems in aqueous phase；
(3) preparation of composite
Nano layered double hydroxides and nanogold are placed in distilled water, nano layered double hydroxides and nanogold
Mass ratio 20：1~1：1, in N2Stirring at normal temperature 24h under atmosphere, using nano layered double hydroxides anion it is commutative
Property, the nanogold of the negative point of surface band is exchanged with original anion in nano layered double hydroxides, be prepared and receive
Rice gold cladding layered double-hydroxide composite.
Nanogold cladding layered double-hydroxide composite can apply to medicine delivery, can modify amino, aldehyde radical,
Antibody, aglucon are to improve target-oriented drug.By taking antineoplastic adriamycin as an example, layered double-hydroxide is coated using nanogold
Composite carries, and adriamycin takes 10mg, 30mg respectively with composite drug-loaded system, the physical mixed in 20mL deionized waters, magnetic
After power stirs 24 hours, centrifuge 2 times, remove supernatant, take precipitation lyophilized.By ultra-violet analysis, the load medicine of adriamycin in medicine-carried system
Measure as 25.4%.
Compared with prior art, the composite drug-loaded system that is prepared of the present invention has pH sensitiveness, high drug load, in vivo
Field cyclicity, surface potential positive and negative can be modified, and surface can link aglucon, antibody, amination, carboxylated, aldehyde radical, for medicine
Carrier, reach the double action of targeting and sustained release in vivo, improve circulation time, drug availability, medicine target inside medicine
Tropism.
By taking antineoplastic adriamycin as an example, (4 μ g/mL) handles brain cancer cell 24 hours under comparable sodium, nanogold bag
After covering layered double-hydroxide composite load medicine, its lethality to tumour can bring up to original 2 times.In Mice Body
Interior, nanogold cladding layered double-hydroxide composite can improve the ability that adriamycin passes through blood-brain barrier.
Brief description of the drawings
Fig. 1 is the Electronic Speculum shape appearance figure of nano layered double hydroxides；
Fig. 2 is the Electronic Speculum shape appearance figure of nanogold；
Fig. 3 is the Electronic Speculum shape appearance figure of composite；
Fig. 4 is the dynamic light scattering diagram of composite；
Fig. 5 is the ultraviolet-visible absorption spectroscopy figure of composite；
Fig. 6 is the Zeta potential analysis chart of composite；
Fig. 7 is the biocompatible cell toxicity test figure of composite；
Fig. 8 is that extracorporeal anti-tumor toxicity test compares figure；
Fig. 9 is the distribution map of medicine in the tissue.
Embodiment
Nanogold coats layered double-hydroxide composite, is core-shell structure, outside is enclosed with nano Au particle
Double-hydroxide particle, wherein, the average grain diameter of nano Au particle is less than 5nm, and the particle diameter of double-hydroxide particle is 20-
200nm.The content of nanogold is 10 in composite-5mol/L。
Contain bivalent metal ion and trivalent metal ion in double-hydroxide, interlayer contains anion.Divalent metal
Ion can be Mg2+、Mn2+、Fe2+、Co2+、Ni2+、Cu2+Or Zn2+Middle one or two, trivalent metal ion can be Al3+、
Cr3+、Mn3+、Fe3+、Co3+Or Ni3+Middle one or two, the anion that interlayer contains are OH-、CO3 2-、SO4 2-、Cl-Or NO3 -In
One or two.
Nanogold coats the preparation method of layered double-hydroxide composite, using following steps：
(1) preparation of nano layered double hydroxides
A, prepare salt containing bivalent metal ion and trivalent metal ion salts solution, bivalent metal ion salt and trivalent metal from
Mol ratio between alite is 1：3；
B, NaOH solution is configured and in N2The lower 60 DEG C of stirrings 10min of atmosphere；
C, step a solution is added drop-wise in step b solution, N2Lower 60 DEG C of atmosphere continues to stir 3h；
D, sample taking-up will be obtained after reaction, is cleaned and centrifuged 3 times repeatedly using distilled water after centrifugation, then be placed in hydro-thermal
Kettle, 100 DEG C of reaction 16h；
E, the sample centrifugal treating that will be obtained, supernatant is removed, is placed in vacuum drying chamber 50 DEG C and is completely dried 48 hours
After take out, be placed in grind into powder in mortar, obtain nano layered double hydroxides；
(2) preparation of nanogold
A, four n-octyl ammonium bromides, lauryl amine, gold chloride are dissolved in toluene, are at room temperature added to sodium borohydride acutely
In the above-mentioned mixed solution of stirring, four n-octyl ammonium bromides, lauryl amine, gold chloride, the mol ratio of sodium borohydride are 0.2-0.3：
0.5-0.7：0.4-0.6：1-3, progress high speed centrifugation obtains oil-soluble nanogold after mixing 2h.
B, gained nanogold is dissolved in chloroform, with molecular weight 2000, the functional polyethylene glycol HS- containing sulfydryl and carboxyl
PEG-COOH modified nano golds surface, reacts 24h at room temperature, obtains stable 5nm nanogold systems in aqueous phase；
(3) preparation of composite
Nano layered double hydroxides and nanogold are placed in distilled water, nano layered double hydroxides and nanogold
Mass ratio 20：1~1：1, in N2Stirring at normal temperature 24h under atmosphere, using nano layered double hydroxides anion it is commutative
Property, the nanogold of the negative point of surface band is exchanged with original anion in nano layered double hydroxides, be prepared and receive
Rice gold cladding layered double-hydroxide composite.
Nanogold cladding layered double-hydroxide composite can apply to medicine delivery, can modify amino, aldehyde radical,
Antibody, aglucon are to improve target-oriented drug.By taking antineoplastic adriamycin as an example, layered double-hydroxide is coated using nanogold
Composite carries, and adriamycin takes 10mg, 30mg respectively with composite drug-loaded system, the physical mixed in 20mL deionized waters, magnetic
After power stirs 24 hours, centrifuge 2 times, remove supernatant, take precipitation lyophilized.By ultra-violet analysis, the load medicine of adriamycin in medicine-carried system
Measure as 25.4%.
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
The preparation of nano layered double hydroxides
Step a：Prepare MgCl2·6H2O (0.6099g, 0.003mol) and AlCl3·9H2O (0.2414g, 0.001mol)
The common 10mL of metal mixed salting liquid
Step b：By the NaOH solution that 40mL concentration is 0.0006mol, make it in N2Stirred 10 minutes at lower 60 DEG C of atmosphere
Step c：Step a solution is added drop-wise in step b solution, N260 degree are stirred 3 hours under atmosphere.
Step d：Sample is taken out after reaction, centrifuges, uses ddH2O water is cleaned, centrifuged three times repeatedly, is transferred to water heating kettle,
Baking oven is placed in, 100 DEG C are reacted 16 hours.
Step e：Sample is centrifuged, removes supernatant, be placed in vacuum drying chamber 50 DEG C be completely dried 48 hours after by its
Take out, be placed in grind into powder in mortar, produce sample, its Electronic Speculum shape appearance figure is as shown in Figure 1.
Embodiment 2
The preparation of nanogold.
Prepare four n-octyl ammonium bromides (136.7mg, 0.25mmol), lauryl amine (111.2mg, 0.6mmol), gold chloride
(218.3mg, 0.53mmol) is dissolved in 5mL toluene.At room temperature, sodium borohydride (75.6mg, 2mmol) is added to and acutely stirred
High speed centrifugation, which is carried out, in the above-mentioned solution mixed, after 2 hours obtains oil-soluble nanogold.Gained nanogold is dissolved in 3mL chloroforms,
Received with functional polyethylene glycol HS-PEG-COOH (2000g/mol, 80mg, 40 μm of ol of the molecular weight) modifications containing sulfydryl and carboxyl
Rice gold surface, reacts 24 hours at room temperature, can obtain in aqueous phase stable 5nm nanogold systems, for LDH phase interactions
With, its Electronic Speculum shape appearance figure is as shown in Figure 2.
Embodiment 3
The preparation of LDH@Au nano composite materials
LDH is prepared by 1/5 system of example 1, (8000rpm, 40 minutes) is collected by centrifugation in hydro-thermal and 200 μ L nanogold are molten
In liquid (1.36*10-5mol/L), it is diluted in jointly in 10mL distilled waters (nitrogen row carbon dioxide).Stirring at normal temperature 24 hours, profit
With the interchangeability of LDH anion, the nanogold of the negative point of surface band is exchanged with original anion in main body, generateLDH@Au, its Electronic Speculum shape appearance figure, dynamic light scattering diagram, ultraviolet-visible absorption spectroscopy figure and Zeta potential analysis chart are respectively such as
Shown in Fig. 3-6, in Fig. 4 (a), 20nm or so is that the peak, 100nm or so of nanogold is LDH peak.(b) number is distributed
Grain-size graph, because the number of nanogold is far longer than LDH, therefore LDH peak is displayed without on the figure.
Embodiment 4
The experiment of LDH@Au vitro cytotoxicities (prepare 96 orifice plate one (5000 cells/well) of U87 cells, be divided into 8 groups,
It is separately added into the solution of the composite, final concentration is respectively 5ug/ml, 10ug/ml, 20ug/ml, 40ug/ml, 80ug/ml,
160ug/ml, 320ug/ml and the contrast groups for being not added with composite, every group of parallel laboratory test group 5,24h are incubated with cell jointly,
Add MTT and test its cell survival rate), biocompatible cell toxicity test figure is as shown in Figure 7.It can be seen that simple material exists
Do not have significant cytotoxicity in the range of 80ug/ml.
Embodiment 5
After LDH@Au carry adriamycin, extracorporeal anti-tumor toxicity test (the orifice plate bed board of SH-SY5Y brain cancer cells 6, divides per hole
Not Jia Ru drug alone, LDH@Au and LDH@Au-DOX solution, final concentration is respectively 0.5ug/ml, 1ug/ml, 2ug/ml,
4ug/ml, every group of parallel laboratory test group 5,24h is incubated with cell jointly, and antitumor activity is analyzed by apoptosis detection kit).
From figure 8, it is seen that under 4 μ g/mL concentration, the cell of LDH@Au-DOX processing has 67% generation apoptosis or death, and DOX
The cell of processing only has 39% generation apoptosis or death.
Embodiment 6
Respectively with DOX and LDH Au-DOX10mg/ml processing tumor-bearing mices, died suddenly at 24 hours mouse, goes respectively each
Organ and tumour, after homogenate, by acetonitrile extraction medicine, drug concentration is then detected by HPLC, while survey each homogenate
Protein concentration, calculate analysis medicine Tissue distribution.As seen from Figure 9, LDH@Au can improve DOX in tumor tissues
Enriched concentration, while DOX can be helped to pass through blood-brain barrier, contribute to the delivery vehicles of cancer of the brain medicine the most anti-.
Embodiment 7
Nanogold coats layered double-hydroxide composite, is core-shell structure, outside is enclosed with nano Au particle
Double-hydroxide particle, the average grain diameter of nano Au particle are less than 5nm, and the particle diameter of double-hydroxide particle is 20nm.Compound
The content of nanogold is 10 in material-5mol/L。
Contain bivalent metal ion and trivalent metal ion in double-hydroxide, interlayer contains anion.In the present embodiment,
Bivalent metal ion is Mg2+, trivalent metal ion Al3+, the anion that interlayer contains is Cl-。
Nanogold coats the preparation method of layered double-hydroxide composite, using following steps：
(1) preparation of nano layered double hydroxides
A, MgCl is prepared2Salt and AlCl3Salting liquid, MgCl2Salt and AlCl3Mol ratio between salt is 1：3；
B, NaOH solution is configured and in N2The lower 60 DEG C of stirrings 10min of atmosphere；
C, step a solution is added drop-wise in step b solution, N2Lower 60 DEG C of atmosphere continues to stir 3h；
D, sample taking-up will be obtained after reaction, is cleaned and centrifuged 3 times repeatedly using distilled water after centrifugation, then be placed in hydro-thermal
Kettle, 100 DEG C of reaction 16h；
E, the sample centrifugal treating that will be obtained, supernatant is removed, is placed in vacuum drying chamber 50 DEG C and is completely dried 48 hours
After take out, be placed in grind into powder in mortar, obtain nano layered double hydroxides；
(2) preparation of nanogold
A, four n-octyl ammonium bromides, lauryl amine, gold chloride are dissolved in toluene, are at room temperature added to sodium borohydride acutely
In the above-mentioned mixed solution of stirring, four n-octyl ammonium bromides, lauryl amine, gold chloride, the mol ratio of sodium borohydride are 0.2：0.5：
0.4：1, progress high speed centrifugation obtains oil-soluble nanogold after mixing 2h.
B, gained nanogold is dissolved in chloroform, with molecular weight 2000, the functional polyethylene glycol HS- containing sulfydryl and carboxyl
PEG-COOH modified nano golds surface, reacts 24h at room temperature, obtains stable 5nm nanogold systems in aqueous phase；
(3) preparation of composite
Nano layered double hydroxides and nanogold are placed in distilled water, nano layered double hydroxides and nanogold
Mass ratio 20：1, in N2Stirring at normal temperature 24h under atmosphere, using the interchangeability of the anion of nano layered double hydroxides, make
The nanogold of the negative point of surface band exchanges with original anion in nano layered double hydroxides, and nanogold bag is prepared
Cover layered double-hydroxide composite.
Nanogold cladding layered double-hydroxide composite can apply to medicine delivery, can modify amino, aldehyde radical,
Antibody, aglucon are to improve target-oriented drug.By taking antineoplastic adriamycin as an example, layered double-hydroxide is coated using nanogold
Composite carries, and adriamycin takes 10mg, 30mg respectively with composite drug-loaded system, the physical mixed in 20mL deionized waters, magnetic
After power stirs 24 hours, centrifuge 2 times, remove supernatant, take precipitation lyophilized.By ultra-violet analysis, the load medicine of adriamycin in medicine-carried system
Measure as 25.4%.
Embodiment 8
Nanogold coats layered double-hydroxide composite, is core-shell structure, outside is enclosed with nano Au particle
Double-hydroxide particle, the average grain diameter of nano Au particle are less than 5nm, and the particle diameter of described double-hydroxide particle is 100nm.
The content of nanogold is 10 in composite-5mol/L。
Contain Mg in double-hydroxide2+、Mn2+Metal ion and Fe3+、Co3+Metal ion, interlayer contain CO3 2-、SO4 2-It is cloudy
Ion.
Nanogold coats the preparation method of layered double-hydroxide composite, using following steps：
(1) preparation of nano layered double hydroxides
A, prepare salt containing bivalent metal ion and trivalent metal ion salts solution, bivalent metal ion salt and trivalent metal from
Mol ratio between alite is 1：3；
B, NaOH solution is configured and in N2The lower 60 DEG C of stirrings 10min of atmosphere；
C, step a solution is added drop-wise in step b solution, N2Lower 60 DEG C of atmosphere continues to stir 3h；
D, sample taking-up will be obtained after reaction, is cleaned and centrifuged 3 times repeatedly using distilled water after centrifugation, then be placed in hydro-thermal
Kettle, 100 DEG C of reaction 16h；
E, the sample centrifugal treating that will be obtained, supernatant is removed, is placed in vacuum drying chamber 50 DEG C and is completely dried 48 hours
After take out, be placed in grind into powder in mortar, obtain nano layered double hydroxides；
(2) preparation of nanogold
A, four n-octyl ammonium bromides, lauryl amine, gold chloride are dissolved in toluene, are at room temperature added to sodium borohydride acutely
In the above-mentioned mixed solution of stirring, four n-octyl ammonium bromides, lauryl amine, gold chloride, the mol ratio of sodium borohydride are 0.25：0.6：
0.5：2, progress high speed centrifugation obtains oil-soluble nanogold after mixing 2h.
B, gained nanogold is dissolved in chloroform, with molecular weight 2000, the functional polyethylene glycol HS- containing sulfydryl and carboxyl
PEG-COOH modified nano golds surface, reacts 24h at room temperature, obtains stable 5nm nanogold systems in aqueous phase；
(3) preparation of composite
Nano layered double hydroxides and nanogold are placed in distilled water, nano layered double hydroxides and nanogold
Mass ratio 10：1, in N2Stirring at normal temperature 24h under atmosphere, using the interchangeability of the anion of nano layered double hydroxides, make
The nanogold of the negative point of surface band exchanges with original anion in nano layered double hydroxides, and nanogold bag is prepared
Cover layered double-hydroxide composite.
Nanogold cladding layered double-hydroxide composite can apply to medicine delivery, can modify amino, aldehyde radical,
Antibody, aglucon are to improve target-oriented drug.By taking antineoplastic adriamycin as an example, layered double-hydroxide is coated using nanogold
Composite carries, and adriamycin takes 10mg, 30mg respectively with composite drug-loaded system, the physical mixed in 20mL deionized waters, magnetic
After power stirs 24 hours, centrifuge 2 times, remove supernatant, take precipitation lyophilized.By ultra-violet analysis, the load medicine of adriamycin in medicine-carried system
Measure as 25.4%.
Embodiment 9
Nanogold coats layered double-hydroxide composite, is core-shell structure, outside is enclosed with nano Au particle
Double-hydroxide particle, the average grain diameter of nano Au particle are less than 5nm, and the particle diameter of double-hydroxide particle is 200nm.Composite wood
The content of nanogold is 10 in material-5mol/L.Contain bivalent metal ion and trivalent metal ion in double-hydroxide, interlayer contains
There is anion.Bivalent metal ion is Mn2+、Cu2+, trivalent metal ion Cr3+, the anion that interlayer contains is OH-、NO3 -。
Nanogold coats the preparation method of layered double-hydroxide composite, using following steps：
(1) preparation of nano layered double hydroxides
A, prepare salt containing bivalent metal ion and trivalent metal ion salts solution, bivalent metal ion salt and trivalent metal from
Mol ratio between alite is 1：3；
B, NaOH solution is configured and in N2The lower 60 DEG C of stirrings 10min of atmosphere；
C, step a solution is added drop-wise in step b solution, N2Lower 60 DEG C of atmosphere continues to stir 3h；
D, sample taking-up will be obtained after reaction, is cleaned and centrifuged 3 times repeatedly using distilled water after centrifugation, then be placed in hydro-thermal
Kettle, 100 DEG C of reaction 16h；
E, the sample centrifugal treating that will be obtained, supernatant is removed, is placed in vacuum drying chamber 50 DEG C and is completely dried 48 hours
After take out, be placed in grind into powder in mortar, obtain nano layered double hydroxides；
(2) preparation of nanogold
A, four n-octyl ammonium bromides, lauryl amine, gold chloride are dissolved in toluene, are at room temperature added to sodium borohydride acutely
In the above-mentioned mixed solution of stirring, four n-octyl ammonium bromides, lauryl amine, gold chloride, the mol ratio of sodium borohydride are 0.3：0.7：
0.6：3, progress high speed centrifugation obtains oil-soluble nanogold after mixing 2h.
B, gained nanogold is dissolved in chloroform, with molecular weight 2000, the functional polyethylene glycol HS- containing sulfydryl and carboxyl
PEG-COOH modified nano golds surface, reacts 24h at room temperature, obtains stable 5nm nanogold systems in aqueous phase；
(3) preparation of composite
Nano layered double hydroxides and nanogold are placed in distilled water, nano layered double hydroxides and nanogold
Mass ratio 1：1, in N2Stirring at normal temperature 24h under atmosphere, using the interchangeability of the anion of nano layered double hydroxides, make table
The nanogold of the negative point of face band exchanges with original anion in nano layered double hydroxides, and nanogold cladding is prepared
Layered double-hydroxide composite.
Nanogold cladding layered double-hydroxide composite can apply to medicine delivery, can modify amino, aldehyde radical,
Antibody, aglucon are to improve target-oriented drug.By taking antineoplastic adriamycin as an example, layered double-hydroxide is coated using nanogold
Composite carries, and adriamycin takes 10mg, 30mg respectively with composite drug-loaded system, the physical mixed in 20mL deionized waters, magnetic
After power stirs 24 hours, centrifuge 2 times, remove supernatant, take precipitation lyophilized.By ultra-violet analysis, the load medicine of adriamycin in medicine-carried system
Measure as 25.4%.
Claims (4)
1. nanogold coats the preparation method of layered double-hydroxide composite, it is characterised in that this method uses following step
Suddenly：
（1）The preparation of nano layered double hydroxides
A, salt containing bivalent metal ion and trivalent metal ion salts solution, bivalent metal ion salt and trivalent metal ion salts are prepared
Between mol ratio be 1：3；
B, NaOH solution is configured and in N2The lower 60 DEG C of stirrings 10min of atmosphere；
C, step a solution is added drop-wise in step b solution, N2Lower 60 DEG C of atmosphere continues to stir 3h；
D, sample taking-up will be obtained after reaction, is cleaned and centrifuged 3 times repeatedly using distilled water after centrifugation, then is placed in water heating kettle, 100
DEG C reaction 16h；
E, the sample centrifugal treating that will be obtained, remove supernatant, be placed in vacuum drying chamber 50 DEG C be completely dried 48 hours after take
Go out, be placed in grind into powder in mortar, obtain nano layered double hydroxides；
（2）The preparation of nanogold
A, four n-octyl ammonium bromides, lauryl amine, gold chloride are dissolved in toluene, sodium borohydride are added to be stirred vigorously at room temperature
Above-mentioned mixed solution in, four n-octyl ammonium bromides, lauryl amine, gold chloride, the mol ratio of sodium borohydride are 0.2-0.3：0.5-
0.7：0.4-0.6：1-3, progress high speed centrifugation obtains oil-soluble nanogold after mixing 2h；
B, gained nanogold is dissolved in chloroform, with molecular weight 2000, the functional polyethylene glycol HS-PEG- containing sulfydryl and carboxyl
COOH modified nano golds surface, reacts 24h at room temperature, obtains stable 5nm nanogold systems in aqueous phase；
（3）The preparation of composite
Nano layered double hydroxides and nanogold are placed in distilled water, the quality of nano layered double hydroxides and nanogold
Than 20：1~1：1, in N2Stirring at normal temperature 24h under atmosphere, using the interchangeability of the anion of nano layered double hydroxides, make
The nanogold of the negative point of surface band exchanges with original anion in nano layered double hydroxides, and nanogold bag is prepared
Cover layered double-hydroxide composite；
The composite is core-shell structure, and outside is enclosed with the double-hydroxide particle of nano Au particle, described nanogold
The average grain diameter of particle is less than 5nm, and the particle diameter of described double-hydroxide particle is 20-200nm.
2. the preparation method of nanogold cladding layered double-hydroxide composite as claimed in claim 1, it is characterised in that
The content of nanogold is 10 in composite-5mol/L。
3. the preparation method of nanogold cladding layered double-hydroxide composite as claimed in claim 1, it is characterised in that
Contain bivalent metal ion and trivalent metal ion in double-hydroxide, interlayer contains anion.
4. the preparation method of nanogold cladding layered double-hydroxide composite as claimed in claim 3, it is characterised in that
Described bivalent metal ion is Mg2+、Mn2+、Fe2+、Co2+、Ni2+、Cu2+Or Zn2+Middle one or two, trivalent metal ion
For Al3+、Cr3+、Mn3+、Fe3+、Co3+Or Ni3+Middle one or two, the anion that interlayer contains are OH-、CO3 2-、SO4 2-、Cl-
Or NO3 -One or both of.
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