CN115282290B - PH response Au@ZIF-8 aqueous phase preparation method - Google Patents
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Abstract
The invention discloses a pH response Au@ZIF-8 water phase preparation method, which comprises the following steps: slowly dripping the soluble zinc salt aqueous solution into the 2-methylimidazole aqueous solution, mixing and reacting until the mixed solution layer is milky, centrifuging and cleaning, and dispersing in deionized water to obtain a ZIF-8 aqueous solution; HAuCl 4 Adding MSA into ZIF-8 water solution, reacting to obtain MSA-HAuCl 4 ZIF-8 solution; naBH is carried out 4 Adding aqueous solution to MSA-HAuCl 4 And (3) in the @ ZIF-8 solution, obtaining Au@ZIF-8 after the reaction. The Au@ZIF-8 is prepared by adopting the water phase preparation method, so that the defects that the biocompatibility and cytotoxicity are influenced by the use of an organic solvent in the traditional preparation method are avoided; the Au@ZIF-8 prepared by the method improves biocompatibility, reduces cytotoxicity and is beneficial to the application of subsequent biological layers; and the yield of the obtained product is high, the nano Au load is high, the particle size is uniform and stable, and the process is simple and nontoxic.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a pH response Au@ZIF-8 aqueous phase preparation method.
Background
Metal organicThe framework material (MOFs for short) is composed of metal ions and organic ligands, and has the characteristics of multiple components, simple synthesis, easy surface functionalization, large specific surface area, adjustable porosity, controllable biocompatibility and the like. ZIF-8 (Zeolitic Imidazolate Framework-8, zeolite imidazole framework material) is one of MOFs material due to Zn 2+ And imidazole ligands have been widely studied due to their ease of preparation and regulation. ZIF-8 is a tumor microenvironment reactive drug carrier, and has potential application value due to higher drug loading capacity, sensitive pH response release and other functions, and has very obvious advantages in the field of tumor drug delivery. Meanwhile, auNPs (also called gold nanoparticles) is a common nano-drug for tumor diagnosis and treatment, and is widely studied as a drug delivery carrier.
In recent years, more and more scientists have found that adsorption of small-sized metal nanoparticles onto the surface of ZIF-8 or embedding into the cavities of ZIF-8 imparts their photo-thermal properties or bio-imaging application characteristics, such as au@zif-8 for pH-responsive release drugs for tumors and tumor imaging techniques. However, most of the current preparation methods of Au@ZIF-8 are carried out by using organic solvents such as methanol, and the problems of solvent residue, cytotoxicity, poor biocompatibility and the like are easily caused. Therefore, the development of a method for preparing Au@ZIF-8 by water phase stabilization has particularly important practical application significance.
Disclosure of Invention
The invention aims to provide a pH response Au@ZIF-8 aqueous phase preparation method which is used for solving the problems of easiness in causing solvent residues, cytotoxicity, poor biocompatibility and the like when an organic solvent is used for preparing Au@ZIF-8 in the prior art.
In order to solve the technical problems, the invention provides a pH response Au@ZIF-8 aqueous phase preparation method, which comprises the following steps: slowly dripping the soluble zinc salt aqueous solution into the 2-methylimidazole aqueous solution, mixing and reacting until the mixed solution layer is milky, centrifuging and cleaning, and dispersing in deionized water to obtain a ZIF-8 aqueous solution; HAuCl 4 Adding MSA into ZIF-8 water solution, reacting to obtain MSA-HAuCl 4 ZIF-8 solventA liquid; naBH is carried out 4 Adding aqueous solution to MSA-HAuCl 4 And (3) in the @ ZIF-8 solution, obtaining Au@ZIF-8 after the reaction.
Preferably, zn in the soluble zinc salt during the preparation of the ZIF-8 aqueous solution 2+ The molar ratio of the catalyst to the 2-methylimidazole is 1:70.
Preferably, the stirring speed of the mixing reaction during the preparation of the ZIF-8 aqueous solution is 1000rpm.
Preferably, the soluble zinc salt includes, but is not limited to, any one or more of zinc nitrate, zinc acetate.
Wherein MSA-HAuCl 4 The @ ZIF-8 solution is a ZIF-8 with an outer surface loaded with HAuCl 4 And an aqueous solution of MSA.
Preferably, MSA-HAuCl 4 HAuCl in preparation process of @ ZIF-8 solution 4 The volume ratio of MSA to ZIF-8 is 1:1: (50-200).
Preferably, the concentration of MSA is 0.3mg/mL.
Preferably, during the preparation of Au@ZIF-8, MSA-HAuCl 4 HAuCl in @ ZIF-8 solution 4 With NaBH 4 The volume ratio is 1: (2-4).
Preferably, naBH 4 The concentration of (C) was 0.5mg/mL.
The Au@ZIF-8 is an aqueous solution with the outer surface of the ZIF-8 loaded with nano Au and MSA, and the Au@ZIF-8 is applied to pH response targeted release of anti-tumor drugs and tumor imaging drugs.
The beneficial effects of the invention are as follows: compared with the prior art, the invention provides the pH response Au@ZIF-8 water phase preparation method, and the Au@ZIF-8 is prepared by adopting the water phase preparation method, so that the defects that the biocompatibility and cytotoxicity are influenced by the use of an organic solvent in the traditional preparation method are avoided; the Au@ZIF-8 prepared by the method improves biocompatibility, reduces cytotoxicity and is beneficial to the application of subsequent biological layers; and the yield of the obtained product is high, the nano Au load is high, the particle size is uniform and stable, and the process is simple and nontoxic.
Drawings
FIG. 1 is a graph showing particle size distribution of ZIF-8 and Au@ZIF-8 prepared in example 1 of the present invention;
FIG. 2 is MSA-HAuCl in examples 2 and 3 of the present invention 4 Particle size-time change diagram of Au@ZIF-8 under different concentrations of @ ZIF-8;
FIG. 3 is a TEM image of ZIF-8 prepared in example 1 of the present invention;
FIG. 4 is a TEM image of MSA-AuNPs@ZIF-8 prepared in example 1 of the present invention;
FIG. 5 is a graph showing the pH response of MSA-AuNPs@ZIF-8 prepared in example 1 of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
The invention provides a pH response Au@ZIF-8 water phase preparation method, which comprises the following steps:
(1) Slowly dripping the soluble zinc salt aqueous solution into the 2-methylimidazole aqueous solution, mixing and reacting until the mixed solution layer is milky, centrifuging and cleaning, and dispersing in deionized water to obtain the ZIF-8 aqueous solution. In this step, zn in the soluble zinc salt 2+ The molar ratio of the zinc salt to the 2-methylimidazole to the water is 1:70:1238, the soluble zinc salt and the 2-methylimidazole are respectively dissolved in a proper amount of deionized water, and then the mixture is stirred and mixed for reaction until the solution is almost milky white, after stirring for 5min, the product is centrifugally collected, washed by the deionized water for a plurality of times, and then dispersed in a proper amount of deionized water to obtain ZIF-8 aqueous solution; in this embodiment, the stirring speed of the mixing reaction is preferably 1000rpm, the centrifugation speed is preferably 8000rpm, and the soluble zinc salt is preferably zinc nitrate.
(2) HAuCl 4 Adding MSA into ZIF-8 water solution, reacting to obtain MSA-HAuCl 4 ZIF-8 solution. In this step, HAuCl 4 The volume ratio of MSA to ZIF-8 is 1:1: (50-200), taking HAuCl 4 And MSA-oneAdding the ZIF-8 aqueous solution obtained in the step (1), stirring for 5min to obtain HAuCl 4 Simultaneously loading MSA and ZIF-8 to obtain MSA-HAuCl 4 ZIF-8 solution. In the present embodiment, HAuCl 4 Preferably 1 wt.%, the concentration of MSA is preferably 0.3mg/mL, MSA being an abbreviation for thiomalic acid.
(3) NaBH is carried out 4 Adding aqueous solution to MSA-HAuCl 4 And (3) in the @ ZIF-8 solution, obtaining Au@ZIF-8 after reaction, wherein the Au@ZIF-8 prepared from the water phase is applied to pH response targeted release of the antitumor drug and the tumor imaging drug. In this step, MSA-HAuCl 4 HAuCl in @ ZIF-8 solution 4 With NaBH 4 The volume ratio is 1: (2-4) the obtained NaBH 4 Adding the aqueous solution to MSA-HAuCl in step (2) 4 ZIF-8 solution, which reacts rapidly to become red, is stirred for 5min to make MSA-HAuCl 4 The @ ZIF-8 is reduced into MSA-AuNPs @ ZIF-8, wherein AuNPs represent gold nanoparticles, and a final product is recorded as Au @ ZIF-8, and the structure is that nano Au and MSA are simultaneously loaded on the outer surface of the ZIF-8; in the present embodiment, naBH 4 The concentration of (C) was 0.5mg/mL.
The product prepared by the above-described pH-responsive Au@ZIF-8 aqueous phase preparation method is characterized by a specific example.
Example 1
The specific steps for preparing Au@ZIF-8 in this example are as follows:
(1) 5.748g of 2-methylimidazole was dissolved in 20mL of deionized water, and 0.2975g of Zn (NO 3 ) 2 · 6 H 2 O was dissolved in 2.28mL deionized water; the Zn (NO) 3 ) 2 · 6 H 2 The O solution was slowly added dropwise to the 2-methylimidazole solution, and after mixing the two solutions, the solution became milky immediately, and after stirring for 5min, the product was collected by centrifugation at 8000rpm, washed several times with deionized water, and then dispersed in 20mL of deionized water to give ZIF-8 aqueous solution.
(2) 0.4mL of 1wt% HAuCl was added 4 And 0.4mL of 0.3mg/mL MSA are added into the ZIF-8 water solution, and the mixture is stirred for 5min to react to obtain MSA-HAuCl 4 ZIF-8 solution.
(3) To the MSA-HAuCl 4 0.8mL of NaBH 0.5mg/mL was added to the @ ZIF-8 solution 4 The aqueous solution turns red rapidly, and Au@ZIF-8 sample 1 is obtained after stirring for 5 min.
Example 2
The specific steps for preparing Au@ZIF-8 in this example are as follows:
(1) 5.748g of 2-methylimidazole was dissolved in 20mL of deionized water, and 0.2975g of Zn (NO 3 ) 2 · 6 H 2 O was dissolved in 2.28mL deionized water; the Zn (NO) 3 ) 2 · 6 H 2 The O solution was slowly added dropwise to the 2-methylimidazole solution, and after mixing the two solutions, the solution became milky immediately, and after stirring for 5min, the product was collected by centrifugation at 8000rpm, washed several times with deionized water, and then dispersed in 20mL of deionized water to give ZIF-8 aqueous solution.
(2) 0.2mL of 1wt% HAuCl 4 And 0.2mL of 0.3mg/mL MSA are added into the ZIF-8 water solution, and the mixture is stirred for 5min to react to obtain MSA-HAuCl 4 ZIF-8 solution.
(3) To the MSA-HAuCl 4 0.8mL of NaBH 0.5mg/mL was added to the @ ZIF-8 solution 4 The aqueous solution turns red rapidly, and Au@ZIF-8 sample 2 is obtained after stirring for 5 min.
Example 3
The specific steps for preparing Au@ZIF-8 in this example are as follows:
(1) 5.748g of 2-methylimidazole was dissolved in 20mL of deionized water, and 0.2975g of Zn (NO 3 ) 2 · 6 H 2 O was dissolved in 2.28mL deionized water; the Zn (NO) 3 ) 2 · 6 H 2 The O solution was slowly added dropwise to the 2-methylimidazole solution, and after mixing the two solutions, the solution became milky immediately, and after stirring for 5min, the product was collected by centrifugation at 8000rpm, washed several times with deionized water, and then dispersed in 20mL of deionized water to give ZIF-8 aqueous solution.
(2) 0.1mL of 1wt% HAuCl 4 And 0.1mL of 0.3mg/mL MSA was added to the above ZIF-8 aqueous solution, and stirred for 5min to obtain MSA-HAuCl 4 ZIF-8 solution.
(3) To the MSA-HAuCl 4 0.4mL of NaBH 0.5mg/mL was added to the @ ZIF-8 solution 4 The aqueous solution turns red rapidly, and Au@ZIF-8 sample 3 is obtained after stirring for 5 min.
The particle sizes of ZIF-8 and Au@ZIF-8 in examples 1 to 3 above were tested, wherein the average particle size of ZIF-8 ranged from 85 to 105nm and the average particle size of Au@ZIF-8 ranged from 90 to 110nm. Specifically, the ZIF-8 and the Au@ZIF-8 prepared in the example 1 are selected for particle size distribution statistics, the result is shown in a graph 1, and the appearance of the Au@ZIF-8 is characterized, and the result is shown in a graph 4, so that AuNPs are wrapped in a ZIF framework; meanwhile, the particle size-time change conditions of the ZIF-8 and the Au@ZIF-8 with different concentrations are tested, and the result is shown in a graph 2, so that a stable particle size range can be maintained all the time regardless of an intermediate product ZIF-8 or a final product Au@ZIF-8, and larger particle size fluctuation can not be generated due to time change, and meanwhile, the prepared stable Au@ZIF-8 is tested for pH responsiveness release, and the fact that the solution color becomes black along with the reduction of pH is obviously found out, so that the Au@ZIF-8 with uniform and stable particle size can be obtained by adopting the Au@ZIF-8 water phase preparation method with the pH response; meanwhile, as can be seen from FIG. 5, the response results of Au@ZIF-8 to different pH conditions are obviously different, and the response identification degree of different pH conditions can be improved.
Compared with the prior art, the invention provides the pH response Au@ZIF-8 water phase preparation method, and the Au@ZIF-8 is prepared by adopting the water phase preparation method, so that the defects that the biocompatibility and cytotoxicity are influenced by the use of an organic solvent in the traditional preparation method are avoided; the Au@ZIF-8 prepared by the method improves biocompatibility, reduces cytotoxicity and is beneficial to the application of subsequent biological layers; and the yield of the obtained product is high, the nano Au load is high, the particle size is uniform and stable, and the process is simple and nontoxic.
It should be noted that, the foregoing embodiments all belong to the same inventive concept, and the descriptions of the embodiments have emphasis, and where the descriptions of the individual embodiments are not exhaustive, reference may be made to the descriptions of the other embodiments.
The foregoing examples merely illustrate embodiments of the invention and are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (5)
1. The pH response Au@ZIF-8 aqueous phase preparation method is characterized by comprising the following steps of:
slowly dripping the soluble zinc salt aqueous solution into the 2-methylimidazole aqueous solution, mixing and reacting until the mixed solution layer is milky, centrifuging and cleaning, and dispersing in deionized water to obtain a ZIF-8 aqueous solution;
HAuCl 4 And MSA is added into the ZIF-8 water solution to react to obtain MSA-HAuCl 4 ZIF-8 solution;
NaBH is carried out 4 Adding an aqueous solution to the MSA-HAuCl 4 Obtaining Au@ZIF-8 after reaction in the@ZIF-8 solution;
in the preparation process of the ZIF-8 aqueous solution, zn in the soluble zinc salt 2+ The mol ratio of the water to the 2-methylimidazole to the water is 1:70-1:140;
the MSA-HAuCl 4 In the preparation process of the @ ZIF-8 solution, the HAuCl 4 The volume ratio of MSA to ZIF-8 is 1:1: (50-200); the concentration of MSA is 0.3mg/mL;
in the preparation process of the Au@ZIF-8, the MSA-HAuCl 4 HAuCl in @ ZIF-8 solution 4 With NaBH 4 The volume ratio is 1: (2-4); the NaBH 4 The concentration of (C) was 0.5mg/mL.
2. The method for preparing a pH-responsive au@zif-8 aqueous phase according to claim 1, wherein the stirring speed of the mixing reaction is 1000rpm during the preparation of the ZIF-8 aqueous solution.
3. The aqueous phase preparation method of pH-responsive au@zif-8 according to claim 1, wherein said soluble zinc salt comprises any one or more of zinc nitrate and zinc acetate.
4. The method for preparing a pH responsive Au@ZIF-8 aqueous phase according to claim 1, wherein said MSA-HAuCl 4 The @ ZIF-8 solution is a ZIF-8 with an outer surface loaded with HAuCl 4 And an aqueous solution of MSA.
5. The method for preparing the pH responsive Au@ZIF-8 aqueous phase according to claim 1, wherein the Au@ZIF-8 is an aqueous phase solution of which the outer surface is simultaneously loaded with nano Au and MSA, and the Au@ZIF-8 is applied to pH responsive targeted release of anti-tumor drugs and tumor imaging drugs.
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| CN115282290A (en) | 2022-11-04 |
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