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Solid-phase synthesis method of tris (bipyridine) ruthenium-lysine polymer

A technology for ruthenium terpyridine and solid-phase synthesis, which is applied in the field of solid-phase synthesis of ruthenium terpyridine-lysine polymers, can solve the problem that the degree of polymerization of the product cannot be absolutely uniform, the number of monomers cannot be uniform, and the luminous intensity is inconsistent. and other problems, to achieve the effect of convenient operation, simple synthesis process and simplified reaction operation

Active Publication Date: 2018-03-06
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the polymerization degree of the product obtained by this method cannot be absolutely uniform, the fluctuation range is wide, and the product with a uniform number of monomers cannot be obtained, resulting in inconsistent luminous intensity. The field has been better applied and promoted, and the applicant has developed a method for synthesizing linear ruthenium terpyridine polymers with uniform and controllable molecular weight.

Method used

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  • Solid-phase synthesis method of tris (bipyridine) ruthenium-lysine polymer

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Experimental program
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Effect test

Embodiment 1

[0042] The solid-phase synthesis method of linear terpyridine ruthenium-lysine polymer includes the preparation of gold substrate, synthesis reaction process, solid phase pretreatment process, solid phase polymerization process and product purification process, such as figure 1 As shown, the specific process is as follows:

[0043] (1) Preparation of gold matrix: including pretreatment of negatively charged slides, Au 3+ Adsorption and generation of crystal seeds and formation of gold matrix.

[0044] Slide pretreatment: First, take a clean negatively charged slide and soak it with 1mL acetone for 1-3 minutes to take it out; secondly, rinse it with 1mL isopropanol, and then immerse it in 1mL isopropanol solution for 1-3 minutes ; Finally, remove the negatively charged slides and wash them with 1 mL of methanol, then immerse in 1 mL of methanol for 1-3 minutes.

[0045] Au 3+ Adsorption and generation of crystal seeds: First, take 3mM HAuCl 4 solution 8mL, immerse negativel...

Embodiment 2

[0058] The solid phase synthesis method of dendritic ruthenium terpyridine polymer mainly consists of the preparation of gold substrate, solid phase pretreatment process, solid phase polymerization process, solid phase termination process, synthesis reaction process and product purification process, such as image 3 shown.

[0059] (1) Preparation of gold matrix: including pretreatment of negatively charged slides, Au 3+ Adsorption and generation of crystal seeds and formation of gold matrix.

[0060] Slide pretreatment: First, take a clean negatively charged slide and soak it with 1mL acetone for 1-3 minutes to take it out; secondly, rinse it with 1mL isopropanol, and then immerse it in 1mL isopropanol solution for 1-3 minutes ; Finally, remove the negatively charged slides and wash them with 1 mL of methanol, then immerse in 1 mL of methanol for 1-3 minutes.

[0061] Au 3+ Adsorption and generation of crystal seeds: First, take 3mM HAuCl 4 solution 8mL, immerse negativel...

Embodiment 3

[0075] On the basis of Example 1, the present invention laterally compares a single terpyridine ruthenium-lysine with the bipyridine ruthenium-lysine polymer in Example 1, each taking an equal amount of 1nM terpyridine ruthenium-lysine Acid and bipyridyl ruthenium-lysine polymer (polymerization degree is 100), under the same conditions, detect its electrochemiluminescent intensity, the result is as follows Figure 4 shown. The luminescence intensity of the linear bipyridyl ruthenium-lysine polymer is much higher than that of a single terpyridine ruthenium-lysine, about 90 times. It can be seen that the synthesis method of the linear bipyridyl ruthenium-lysine polymer proposed by the present invention can greatly enhance the luminescence intensity of a single ECL probe, thus providing powerful sensitivity performance for trace analysis based on ECL technology Assure.

[0076] Moreover, the present invention synthesized linear terpyridine ruthenium-lysine polymers with differe...

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Abstract

The invention discloses a solid-phase synthesis method of a tris (bipyridine) ruthenium-lysine polymer. The solid-phase synthesis method comprises the following steps: carrying out a solid-phase pretreatment process on a first reaction substrate, containing lysine, of synthetic raw materials to obtain a thiolated monomer, and then fixing the thiolated monomer with a gold matrix so as to form a second reaction substrate; carrying out a solid phase polymerization process on the second reaction substrate with the first reaction substrate after deaminization protection, after forming a fixed polymer, enabling the gold matrix to fall off from the fixed polymer to obtain a target product, and carrying out a product purification process on the target product to obtain the tris (bipyridine) ruthenium-lysine polymer. The invention initiates a synthetic method for the tris (bipyridine) ruthenium-lysine polymer on the basis of a solid-phase synthesis principle, and a linear or tree-like polymer is obtained by changing the amino protection position of lysine. The degree of polymerization of the obtained tris (bipyridine) ruthenium-lysine polymer is adjustable, the luminous intensity is stableand uniform, and powerful luminous intensity support is provided for a measurement analytic method on the basis of a electrochemical luminescence principle.

Description

technical field [0001] The invention belongs to the technical field of electrochemiluminescent polymer synthesis, and in particular relates to a solid phase synthesis method of terpyridine ruthenium-lysine polymer. Background technique [0002] As a widely used electrochemiluminescent group, ruthenium terpyridyl molecule plays an increasingly important role in the field of immunoassay and molecular diagnosis. However, a single ruthenium terpyridyl molecule cannot provide sufficient luminescence intensity support for trace analysis techniques. Therefore, it is of great significance to develop a new type of linear ruthenium terpyridine polymer with electrochemical amplification function. Inspired by polylysine polymers in the early stage, the applicant constructed a synthesis method of linear terpyridine ruthenium polymerization, and successfully applied it in the field of tumor molecular diagnosis, which has now been authorized (ZL). However, the polymerization degree of th...

Claims

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Application Information

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IPC IPC(8): C08G83/00C08G69/42
CPCC08G69/42C08G83/003C08G83/004
Inventor 黄曦廖玉辉赵钊艳谭青琴
Owner SUN YAT SEN UNIV