Metal nanoprobe applied to mass spectrometry flow technology, preparation method and application
A metal nanoprobe technology, applied in the field of nanoprobes, can solve the problems of limited sensitivity of the detection channel, and achieve the effects of good dispersion, broadened detection channel, and simple chemical synthesis
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Embodiment 1
[0043] In order to obtain Zr-MOF with uniform size and high solvent dispersion, Zr-MOF was synthesized by solvothermal method. ) and reaction time on the particle size and stability of Zr-MOF materials. Through the optimization of conditions, the optimal reaction conditions were determined, and the small-sized UIO-66 crystal structure dispersed stably in aqueous solution was finally synthesized.
[0044] like figure 1As shown, Zr-MOFs with different particle sizes were obtained by adjusting the concentration of the monocarboxylic acid regulators dichloroacetic acid and formic acid and adjusting the time. like Figure 2 to Figure 4 As shown, the change process of the particle size of Zr-MOF under the control of formic acid and the control of dichloroacetic acid is disclosed respectively.
Embodiment 2
[0046] This embodiment discloses the preparation of 30nm Zr-MOF, which specifically includes the following steps:
[0047] Step 1: Preparation of storage solution, specifically: dissolving 210 mg of zirconium chloride in 30 mL of N,N-dimethylamide (DMF), ultrasonically dispersing to complete dissolution to prepare solution 1; dissolving 500 mg of terephthalic acid ( H2BDC) was dissolved in 10 mL of DMF, and ultrasonically dispersed to complete dissolution to prepare storage solution 2; storage solution 1 and storage solution 2 were placed in a 90°C oven to preheat.
[0048] Step 2: Add 3mL of stock solution 1 and 1mL of stock solution 2 to a 10mL glass bottle respectively, vortex to mix well (stock solution 1+2 system), add 393μL and 141μL of formic acid dropwise to the two bottles, and vortex to mix well , placed in an oven at 90°C, and reacted for 6h. A small number of parallel experiments were carried out simultaneously in this step.
[0049] Step 3: After the product was...
Embodiment 3
[0051] like Figure 5 As shown, this example couples the Zr-MOF material to the antibody via the EDC / NHS system.
[0052] 1-(3-Methylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) is a zero-length crosslinker for the coupling of carboxyl groups to primary amines. EDC first reacts with the carboxyl group and forms an amine-reactive O-acylisourea intermediate, which rapidly reacts with the amino group to form an amide bond and liberate the isourea by-product. The intermediate is unstable in aqueous solution, therefore, the two-step coupling method requires N-hydroxysuccinimide (NHS) for stabilization; failure to react with the amine will result in hydrolysis of the intermediate, regeneration of the carboxyl group, and release of the N-substituted urea.
[0053] When using a two-step protein coupling of EDC and NHS or sulfo-NHS, the EDC activation reaction is most efficient at pH 4.5-7.2, and the EDC reaction is usually performed in MES buffer at pH 4.7-6.0. Reactions of ...
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Abstract
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