CN115282290A - pH-responsive Au @ ZIF-8 water phase preparation method - Google Patents
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Abstract
The invention discloses a pH-responsive Au @ ZIF-8 water phase preparation method, which comprises the following steps: slowly dripping soluble zinc salt aqueous solution into 2-methylimidazole aqueous solution, mixing and reacting until the mixed solution layer is milk white, centrifuging, cleaning, dispersing in deionized water,obtaining ZIF-8 aqueous solution; adding HAuCl 4 Adding MSA and the aqueous solution of ZIF-8, and reacting to obtain MSA-HAuCl 4 @ ZIF-8 solution; reacting NaBH 4 Adding the aqueous solution to MSA-HAuCl 4 In the solution of @ ZIF-8, au @ ZIF-8 is obtained after the reaction. The invention adopts the aqueous phase preparation method to prepare Au @ ZIF-8, thereby avoiding the defects of using organic solvent to influence biocompatibility and cytotoxicity in the traditional preparation method; the Au @ ZIF-8 prepared by the method improves the biocompatibility, reduces the cytotoxicity and is beneficial to the application of the subsequent biological layer; and the yield of the obtained product is high, the load of the nano Au is high, the particle size is uniform and stable, and the process is simple and convenient and has no toxicity.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a pH-responsive Au @ ZIF-8 aqueous phase preparation method.
Background
The metal organic framework material (MOFs for short) is composed of metal ions and organic ligands, and has the characteristics of multiple components, simplicity in synthesis, easiness in surface functionalization, large specific surface area, adjustable porosity, controllable biocompatibility and the like. ZIF-8 (full name Zeolite imidazole Framework-8, zeolite imidazole Framework structure material) is one of the materials of MOFs, because of Zn 2+ And imidazole ligands have been extensively studied due to their ease of preparation and manipulation. ZIF-8 is a tumor microenvironment reactive drug carrier, shows potential application value due to higher drug loading capacity and sensitive pH response release and other functions, and has very obvious advantages in the field of tumor drug delivery. Meanwhile, auNPs (also known as gold nanoparticles) are common tumor diagnosis and treatment nano-drugs and are widely researched as drug delivery carriers.
In recent years, more and more scientists have found that small-sized metal nanoparticles are adsorbed on the surface of ZIF-8 or embedded in the cavity of ZIF-8, thereby giving them photothermal properties or characteristics for bioimaging applications, such as Au @ ZIF-8 for pH-responsive drug release in tumors and tumor imaging technology. However, most of the existing methods for preparing Au @ ZIF-8 are prepared by using organic solvents such as methanol and the like, and the problems of solvent residue, low cytotoxicity, poor biocompatibility and the like are easily caused. Therefore, the development of a method for stably preparing Au @ ZIF-8 in an aqueous phase has particularly important practical application significance.
Disclosure of Invention
The invention aims to provide a pH-responsive Au @ ZIF-8 water-phase preparation method, which is used for solving the problems of solvent residue, poor cytotoxicity, poor biocompatibility and the like easily caused when Au @ ZIF-8 is prepared by using an organic solvent in the prior art.
In order to solve the technical problem, the invention provides a pH-responsive Au @ ZIF-8 water phase preparation method, which comprises the following steps: slowly dropwise adding a soluble zinc salt aqueous solution into a 2-methylimidazole aqueous solution, mixing and reacting until a mixed solution layer is milky, centrifuging, cleaning, and dispersing in deionized water to obtain a ZIF-8 aqueous solution; adding HAuCl 4 Adding MSA and the aqueous solution of ZIF-8, and reacting to obtain MSA-HAuCl 4 @ ZIF-8 solution; reacting NaBH 4 Adding the aqueous solution to MSA-HAuCl 4 And 3, in the @ ZIF-8 solution, reacting to obtain Au @ ZIF-8.
Preferably, zn is present in the soluble zinc salt during the preparation of the aqueous ZIF-8 solution 2+ The molar ratio to 2-methylimidazole is 1.
Preferably, the stirring speed of the mixing reaction during the preparation of the aqueous ZIF-8 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 @ ZIF-8 solution is ZIF-8 external surface and loaded with HAuCl 4 And an aqueous solution of MSA.
Preferably, MSA-HAuCl 4 In the preparation of @ ZIF-8 solution, HAuCl 4 The volume ratio of MSA to ZIF-8 is 1: (50-200).
Preferably, the concentration of MSA is 0.3mg/mL.
Preferably, in the preparation of Au @ ZIF-8, MSA-HAuCl 4 @ ZIF-8 solution in HAuCl 4 With NaBH 4 The volume ratio is 1: (2-4).
Preferably, naBH 4 The concentration of (2) was 0.5mg/mL.
The external surface of the Au @ ZIF-8 is simultaneously loaded with nano Au and MSA aqueous solution, and the Au @ ZIF-8 is applied to pH response targeted release antitumor drugs and tumor imaging drugs.
The invention has the beneficial effects that: compared with the prior art, the invention provides the pH-responsive Au @ ZIF-8 aqueous phase preparation method, and the Au @ ZIF-8 is prepared by adopting the aqueous phase preparation method, so that the defects that the biocompatibility and cytotoxicity are influenced by using an organic solvent in the traditional preparation method are overcome; the Au @ ZIF-8 prepared by the method improves biocompatibility, reduces cytotoxicity and is beneficial to application of a subsequent biological layer; and the yield of the obtained product is high, the load of the nano Au is high, the particle size is uniform and stable, and the process is simple and convenient and has no toxicity.
Drawings
FIG. 1 is a graph showing the distribution of particle sizes of ZIF-8 and Au @ ZIF-8 prepared in example 1 of the present invention;
FIG. 2 shows MSA-HAuCl in examples 2 and 3 of the present invention 4 Particle size-time variation graph of Au @ ZIF-8 at 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 change of MSA-AuNPs @ ZIF-8 prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a pH-responsive Au @ ZIF-8 water phase preparation method, which comprises the following steps:
(1) Slowly dripping soluble zinc salt aqueous solution into 2-methylimidazole aqueous solution, mixing and reacting until the mixture is completely dissolvedAnd centrifuging and cleaning the mixed solution layer to disperse in deionized water to obtain the ZIF-8 aqueous solution. In this step, zn is contained in the soluble zinc salt 2+ Dissolving soluble zinc salt and 2-methylimidazole in a proper amount of deionized water respectively at a molar ratio of 1; in the present 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) Adding HAuCl 4 Adding MSA into ZIF-8 aqueous 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: (50-200) taking the HAuCl 4 Adding the ZIF-8 aqueous solution obtained in step (1) together with MSA, and stirring for 5min to allow HAuCl 4 Loading MSA and ZIF-8 on the outer surface simultaneously to obtain MSA-HAuCl 4 @ ZIF-8 solution. In this embodiment, HAuCl 4 Is preferably 1wt%, the concentration of MSA is preferably 0.3mg/mL, MSA being an abbreviation for thiomalic acid.
(3) Reacting NaBH 4 Adding the aqueous solution to MSA-HAuCl 4 In the @ ZIF-8 solution, au @ ZIF-8 is obtained after reaction, and the Au @ ZIF-8 prepared by the aqueous phase is applied to pH response targeted release of antitumor drugs and tumor imaging drugs. In this step, MSA-HAuCl 4 @ ZIF-8 solution in HAuCl 4 With NaBH 4 The volume ratio is 1: (2-4), collecting the NaBH 4 Adding the aqueous solution to MSA-HAuCl in the step (2) 4 @ ZIF-8 solution, which rapidly reacts to become red, and stirring for 5min to make MSA-HAuCl 4 @ ZIF-8 is reduced into MSA-AuNPs @ ZIF-8, auNPs represent gold nanoparticles, the final product is marked as Au @ ZIF-8, and the structure of the gold nanoparticles is that nano Au and MSA are simultaneously loaded on the outer surface of ZIF-8; in this embodiment, naBH 4 The concentration of (2) was 0.5mg/mL.
The product prepared by the above-described pH responsive Au @ ZIF-8 aqueous phase preparation method is characterized by the specific examples below.
Example 1
The specific steps for preparing Au @ ZIF-8 in the embodiment are as follows:
(1) 5.748g of 2-methylimidazole are dissolved in 20mL of deionized water, and 0.2975g of Zn (NO) is added 3 ) 2 · 6 H 2 Dissolving O in 2.28mL of deionized water; adding the above Zn (NO) 3 ) 2 · 6 H 2 And slowly dropwise adding the O solution into the 2-methylimidazole solution, mixing the two solutions, immediately turning the solution into milk white, stirring for 5min, centrifuging at 8000rpm, collecting a product, washing with deionized water for several times, and dispersing in 20mL of deionized water to obtain the ZIF-8 aqueous solution.
(2) 1wt% HAuCl in 0.4mL 4 And 0.4mL of 0.3mg/mL MSA is added into the ZIF-8 aqueous solution, stirred for 5min, and reacted to obtain MSA-HAuCl 4 @ ZIF-8 solution.
(3) To the above MSA-HAuCl 4 0.8mL of 0.5mg/mL NaBH added to the solution of @ ZIF-8 4 The aqueous solution rapidly turned red, and after stirring for 5min, au @ ZIF-8 sample 1 was obtained.
Example 2
The specific steps for preparing Au @ ZIF-8 in the embodiment are as follows:
(1) 5.748g of 2-methylimidazole are dissolved in 20mL of deionized water, and 0.2975g of Zn (NO) is added 3 ) 2 · 6 H 2 Dissolving O in 2.28mL of deionized water; adding the above Zn (NO) 3 ) 2 · 6 H 2 And slowly dropwise adding the O solution into the 2-methylimidazole solution, mixing the two solutions, immediately turning the solution into milk white, stirring for 5min, centrifuging at 8000rpm, collecting a product, washing with deionized water for several times, and dispersing in 20mL of deionized water to obtain the ZIF-8 aqueous solution.
(2) 0.2mL of 1wt% HAuCl 4 Adding 0.2mL of 0.3mg/mL MSA into the ZIF-8 aqueous solution, stirring for 5min, and reacting to obtain MSA-HAuCl 4 @ ZIF-8 solution.
(3) To the above MSA-HAuCl 4 0.8mL of 0.5mg/mL NaBH added to the solution of @ ZIF-8 4 The aqueous solution rapidly turned red, and after stirring for 5min, au @ ZIF-8 sample 2 was obtained.
Example 3
The specific steps for preparing Au @ ZIF-8 in the embodiment are as follows:
(1) 5.748g of 2-methylimidazole are dissolved in 20mL of deionized water, and 0.2975g of Zn (NO) is added 3 ) 2 · 6 H 2 Dissolving O in 2.28mL of deionized water; adding the above Zn (NO) 3 ) 2 · 6 H 2 And slowly dropwise adding the O solution into the 2-methylimidazole solution, mixing the two solutions, immediately turning the solution into milk white, stirring for 5min, centrifuging at 8000rpm, collecting a product, washing with deionized water for several times, and dispersing in 20mL of deionized water to obtain the ZIF-8 aqueous solution.
(2) 1wt% HAuCl in 0.1mL 4 And 0.1mL of 0.3mg/mL MSA is added into the ZIF-8 aqueous solution, stirred for 5min and reacted to obtain MSA-HAuCl 4 @ ZIF-8 solution.
(3) To the above MSA-HAuCl 4 0.4mL of 0.5mg/mL NaBH was added to the @ ZIF-8 solution 4 The aqueous solution rapidly turned red, and after stirring for 5min, au @ ZIF-8 sample 3 was obtained.
The particle sizes of ZIF-8 and Au @ ZIF-8 in examples 1 to 3 were measured, in which the average particle size of ZIF-8 was in the range of 85 to 105nm and the average particle size of Au @ ZIF-8 was in the range of 90 to 110nm. Specifically, the ZIF-8 and Au @ ZIF-8 prepared in the embodiment 1 are selected for carrying out particle size distribution statistics, the result is shown in figure 1, the Au @ ZIF-8 is subjected to morphology characterization, and the result is shown in figure 4, so that AuNPs are wrapped in the ZIF framework; meanwhile, the particle size-time change conditions of ZIF-8 and Au @ ZIF-8 with different concentrations are tested, and the results are shown in figure 2, so that whether the intermediate product ZIF-8 or the final product Au @ ZIF-8 is obtained, a relatively stable particle size range can be maintained all the time, and relatively large particle size fluctuation can not be generated even in time, and similarly, the prepared stable Au @ ZIF-8 is subjected to a pH response release test, and the phenomenon that the color of the solution is blackened along with the reduction of the pH is obviously found out, so that the Au @ ZIF-8 water phase preparation method with the pH response can obtain the Au @ ZIF-8 with uniform and stable particle size; 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 degrees of different pH conditions can be improved.
Compared with the prior art, the invention provides the pH-responsive Au @ ZIF-8 aqueous phase preparation method, and the Au @ ZIF-8 is prepared by adopting the aqueous phase preparation method, so that the defects of influence on biocompatibility and cytotoxicity caused by using an organic solvent in the traditional preparation method are avoided; the Au @ ZIF-8 prepared by the method improves the biocompatibility, reduces the cytotoxicity and is beneficial to the application of the subsequent biological layer; and the yield of the obtained product is high, the load of the nano Au is high, the particle size is uniform and stable, and the process is simple and convenient and has no toxicity.
It should be noted that the above embodiments all belong to the same inventive concept, and the description of each embodiment has its emphasis, and where the description in a particular embodiment is not exhaustive, reference may be made to the description in other embodiments.
The above-mentioned embodiments only express the embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A pH-responsive Au @ ZIF-8 water phase preparation method is characterized by comprising the following steps:
slowly dropwise adding a soluble zinc salt aqueous solution into a 2-methylimidazole aqueous solution, carrying out mixing reaction until a mixed solution layer is milky white, centrifuging, cleaning, and dispersing in deionized water to obtain a ZIF-8 aqueous solution;
adding HAuCl 4 Adding MSA into the ZIF-8 aqueous solution, and reacting to obtain MSA-HAuCl 4 @ ZIF-8 solution;
reacting NaBH 4 Adding an aqueous solution to the MSA-HAuCl 4 In the solution of @ ZIF-8, au @ ZIF-8 is obtained after the reaction.
2. The process for the preparation of a pH-responsive Au @ ZIF-8 aqueous phase as claimed in claim 1, whereinIn that Zn is contained in the soluble zinc salt during the preparation of the ZIF-8 aqueous solution 2+ The molar ratio of the 2-methylimidazole to the water is 1.
3. The method for the preparation of pH-responsive au @ ZIF-8 aqueous phase as claimed in claim 1, wherein the mixing reaction is performed at a stirring speed of 1000rpm during the preparation of the ZIF-8 aqueous solution.
4. The method for the preparation of a pH-responsive au @ zif-8 aqueous phase as claimed in claim 1, wherein the soluble zinc salt comprises any one or more of zinc nitrate, zinc acetate.
5. The pH responsive Au @ ZIF-8 aqueous phase preparation method as claimed in claim 1, wherein the MSA-HAuCl is 4 @ ZIF-8 solution is ZIF-8 external surface and loaded with HAuCl 4 And an aqueous solution of MSA.
6. The pH responsive Au @ ZIF-8 aqueous phase preparation method as claimed in claim 1, wherein the MSA-HAuCl is 4 @ ZIF-8 solution preparation Process, the HAuCl 4 The volume ratio of MSA to ZIF-8 is 1: (50-200).
7. The process for the aqueous phase preparation of pH-responsive au @ zif-8 as claimed in claim 1, wherein the concentration of MSA is 0.3mg/mL.
8. The pH-responsive Au @ ZIF-8 aqueous phase preparation method as claimed in claim 1, wherein the MSA-HAuCl is in the process of preparing the Au @ ZIF-8 4 @ ZIF-8 solution in HAuCl 4 With NaBH 4 The volume ratio is 1: (2-4).
9. The pH-responsive Au @ ZIF-8 aqueous phase preparation method of claim 1, wherein the NaBH is 4 The concentration of (2) was 0.5mg/mL.
10. The pH-responsive Au @ ZIF-8 aqueous phase preparation method as claimed in claim 1, wherein the Au @ ZIF-8 is an aqueous phase solution in which nanometer Au and MSA are simultaneously loaded on the outer surface of the ZIF-8, and the Au @ ZIF-8 is applied to pH-responsive targeted release of antitumor drugs and tumor imaging drugs.
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