his@zif-8/tb 3+ Preparation method of composite material
A composite material, the technology of zinc nitrate hexahydrate, applied in the field of zeolite imidazolate frame composite materials, can solve problems such as undiscovered, and achieve the effects of low detection limit, high water stability and high sensitivity
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Embodiment 1
[0053] The preparation process of the His@ZIF-8 composite material of the present invention is as follows:
[0054] a. Dissolve 3.0 mmol of histidine in 40 mL of deionized water, then add 250 μL of triethylamine into the histidine solution and stir for 5 min.
[0055] b. Dissolve 6.0 mmol of zinc nitrate hexahydrate and 21.0 mmol of 2-methylimidazole in 100 mL and 60 mL of methanol respectively to obtain zinc nitrate hexahydrate solution and 2-methylimidazole solution;
[0056] c. In order to prepare the ZIFs precursor solution, first mix the 2-methylimidazole solution with the histidine solution, and stir for 15 minutes, then add the hexahydrate zinc nitrate solution, stir the above mixed solution at room temperature for 24 hours, and pass through at 7000rpm The product was collected by centrifugation for 5 min, washed with methanol three times repeatedly, and the obtained white powder was dried in an oven at 60 °C.
[0057] The present invention His@ZIF-8 / Tb 3+ The prepara...
Embodiment 2
[0069] The present invention adopts His@ZIF-8 / Tb prepared in Example 1 3+ The composite material was successfully applied to the standard addition method detection of DPA in 10% human urine.
[0070] Specific steps are as follows:
[0071] 1) Filter the human urine sample with a 0.45 μm filter to remove any potential particulate suspension. Recovery experiments were performed by adding three different concentrations (0.5, 1.0 and 5.0 μmol / L) of DPA. Human urine was finally diluted 10-fold in the test solution.
[0072] 2) All the other are as in Example 1.
[0073] As can be seen from Table 1, the recovery rate is in the range of 98.7-103.2%, and the relative standard deviation (n=3) is less than 3%, indicating that the composite material is accurate and precise in detecting DPA in 10% human urine biological samples higher.
Embodiment 3
[0075] The present invention adopts His@ZIF-8 / Tb prepared in Example 1 3+ The composite material was successfully applied to the standard addition method of DPA in 1% bovine serum.
[0076] Specific steps are as follows:
[0077] 1) Use trifluoroacetic acid to hydrolyze the bovine serum sample, remove the protein, centrifuge to obtain the bovine serum treatment solution, and dilute it 10 times with HEPES buffer solution (pH=7.4, 20mmol / L), by adding three different concentrations (0.5, 1.0 and 5.0 μmol / L) of DPA for recovery test. In the test solution, the bovine serum was finally diluted 100 times.
[0078] 2) All the other are as in Example 1.
[0079] As can be seen from Table 1, the recovery rate is in the range of 97.2-102.7%, and the relative standard deviation (n=3) is less than 5%, indicating that the composite material has higher accuracy and precision in detecting DPA in 1% bovine serum samples .
[0080] Table 1 Recovery test results
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