Preparation method of electrochemiluminescence nano illuminant based on aminated bipyridyl ruthenium

A luminescent body and glutamic acid technology, applied in chemiluminescence/bioluminescence, chemical instruments and methods, and electrochemical variables of materials, etc., can solve problems such as difficult solid-state sensing platform, easy aggregation of water phase, and low luminous efficiency of ECL , to achieve the effect of reducing the intensity leakage of illuminants

Active Publication Date: 2020-11-24
ZHEJIANG NORMAL UNIVERSITY
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Problems solved by technology

[0005] Aiming at the shortcomings of the existing ECL of bipyridyl ruthenium and its derivatives, such as low luminous efficiency, easy aggregation in the water phase, unstable intermediates, and difficulty in being directly applied to solid-state sensing platforms, the present invention provides a Ru(bpy) based -NH 2 Preparation method of enhanced ECL luminescent material

Method used

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  • Preparation method of electrochemiluminescence nano illuminant based on aminated bipyridyl ruthenium
  • Preparation method of electrochemiluminescence nano illuminant based on aminated bipyridyl ruthenium
  • Preparation method of electrochemiluminescence nano illuminant based on aminated bipyridyl ruthenium

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Embodiment 1

[0026] A Ru(bpy)-NH based 2 The preparation method of the ECL luminescent body, including the synthesis of Ru / Pd NSs@MIL-101, the synthetic route is as follows figure 1 As shown, the specific steps are as follows:

[0027] Step 1, disperse 0.8g of chromium nitrate nonahydrate, 0.294g of glutamic acid and 0.2g of sodium hydroxide in 15mL of water in one pot. After the dissolution is complete, transfer it to a 25mL reactor and react at 160°C for 12 hours. The resulting solution is passed through MIL-101(Cr) was obtained by centrifuging and washing with a mixed solution of water and methanol at a volume ratio of 1:1, followed by activation at 200°C for 6 hours.

[0028] Step 2, disperse 0.1g MIL-101(Cr) in 20mL water, ultrasonically disperse in ultrapure water, slowly add 0.06g palladium chloride powder to it under magnetic stirring, the mass ratio of the two is 5:3, after stirring for 4 hours Centrifuge to remove unbound palladium chloride. The obtained precipitate was redisp...

Embodiment 2

[0031] A Ru(bpy)-NH based 2 The preparation method of the ECL luminescent body, including the synthesis of Ru / Pd NSs@MIL-101, the synthetic route is as follows figure 1 As shown, the specific steps are as follows:

[0032] Step 1, disperse 0.8g of chromium nitrate nonahydrate, 0.294g of glutamic acid and 0.2g of sodium hydroxide in 10mL of water in one pot. After the dissolution is complete, transfer it to a 50mL reactor and react at 200°C for 18 hours. The resulting solution is passed through MIL-101(Cr) was obtained by centrifuging and washing with a mixed solution of water and methanol at a volume ratio of 1:1, followed by activation at 160° C. for 4 hours.

[0033]Step 2, disperse 0.1g MIL-101(Cr) in 10mL water, ultrasonically disperse in ultrapure water, slowly add 0.1g palladium chloride powder to it under magnetic stirring, the mass ratio of the two is 1:1, after stirring for 6 hours Centrifuge to remove unbound palladium chloride. The resulting precipitate was redis...

Embodiment 3

[0036] A Ru(bpy)-NH based 2 The preparation method of the ECL luminescent body, including the synthesis of Ru / Pd NSs@MIL-101, the synthetic route is as follows figure 1 As shown, the specific steps are as follows:

[0037] Step 1, disperse 0.8g of chromium nitrate nonahydrate, 0.294g of glutamic acid and 0.2g of sodium hydroxide in 5mL of water in one pot, transfer it to a 30mL reactor after the dissolution is complete, and react at 180°C for 14 hours. MIL-101(Cr) was obtained by centrifuging and washing with a mixed solution of water and methanol at a volume ratio of 1:1, followed by activation at 180° C. for 2 hours.

[0038] Step 2, disperse 0.1g MIL-101(Cr) in 15mL water, ultrasonically disperse in ultrapure water, slowly add 0.06g palladium chloride powder to it under magnetic stirring, the mass ratio of the two is 5:3, after stirring for 4 hours Centrifuge to remove unbound palladium chloride. The obtained precipitate was redispersed into 20mL water, added 0.1mL hydra...

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Abstract

The invention relates to a preparation method of an electrochemiluminescence (ECL) nano illuminant based on aminated bipyridyl ruthenium (Ru(bpy)-NH2). The invention provides a preparation method of an enhanced ECL luminescent material based on Ru(bpy)-NH2 in order to overcome the defects that existing bipyridyl ruthenium and derivatives thereof are low in ECL luminescent efficiency, prone to aggregation in a water phase, unstable in intermediate, difficult to be directly applied to a solid-state sensing platform and the like. According to the method, Pd<2+> is subjected to in-situ reduction on the surface of MIL-101(Cr) to synthesize Pd NSs@MIL-101 on the basis of a palladium metal work function, an excited state energy level of Ru(bpy)-NH2 and a principle that excited potentials of the palladium metal work function and the Ru(bpy)-NH2 are close to each other, so that the efficient ECL nanometer illuminant (Ru/Pd NSs@MIL-101) is formed. The prepared material is stable in luminescence,high in strength and simple in biological modification, and can be applied to the solid-state sensing platform.

Description

technical field [0001] The invention belongs to the field of photoelectric detection, and relates to an aminated bipyridyl ruthenium (Ru(bpy)-NH 2 ), a method for preparing an electrochemiluminescent (ECL) nanoluminescent body. Background technique [0002] At present, based on the advantages of zero background interference, simple instrument operation, and high sensitivity, ECL technology has been widely used in in vitro biosensing detection, image signal transduction and other fields. A variety of organic molecules such as luminol, boron-dipyrromethene (BODIPY), and metal-organic compounds have shown their potential for ECL luminescence. Due to the advantages of stable luminous efficiency, low dosage, high cost performance and transparent luminescent mechanism, bipyridyl ruthenium and its derivatives are the most widely used luminescent molecules in ECL biological detection. However, with the rapid development of biomedical technology, it is difficult to match the ECL si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/06C09K11/87G01N21/76G01N27/26
CPCC09K11/02C09K11/06C09K11/87G01N27/26G01N21/76C09K2211/185C09K2211/183
Inventor 袁培新王慧敏王奕雯王爱军冯九菊
Owner ZHEJIANG NORMAL UNIVERSITY
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