Method for preparing solid electrochemical luminescence sensor

A sensor and electrochemical technology, which is applied in the field of preparation of solid-state electrochemiluminescent sensors, can solve the problems of strict raw material requirements, complicated preparation process, and complicated preparation process, and achieve friendly application environment, high preparation efficiency, and simple preparation process Effect

Active Publication Date: 2016-08-31
QINGDAO UNIV
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Problems solved by technology

The Chinese invention patent with the application number of 201410185102.5 discloses a preparation method of a solid-state electrochemiluminescence sensor, preparing nano-gold-silicon dioxide core-shell composite structure nanomaterials doped with ruthenium complexes (Au@SiO 2 -Ru), the composite nanomaterial is fixed on the surface of the glassy carbon electrode to make a reagent-free electrochemiluminescence sensor, although the electrochemiluminescence reagent of the sensor prepared by this method is fixed on the electrode and can be reused, but this preparation method has great influence on the preparation Raw material requirements are strict, the preparation process is complicated, the preparation process is complicated, and it is difficult to produce on a large scale

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  • Method for preparing solid electrochemical luminescence sensor
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Embodiment 2

[0037] In this example, 4-cyano-4-ethyltrithiopentanoic acid (CETP) was functionalized with pyrene to obtain pyrene-functionalized pyrene-functionalized 4-cyano-4-ethyltrithiopentanoic acid ( PCETP) reagent, the specific process is:

[0038] (1) Dissolve 0.5g pyrenemethanol, 0.73g CETP, 0.6383g dicyclohexylcarbodiimide (DCC) and 0.0378g 4-dimethylaminopyridine (DMAP) in 10mL tetrahydrofuran (THF) respectively to obtain a mixture;

[0039] (2) The mixture described in step (1) was stirred and reacted at room temperature for 12 hours, and then filtered to remove solid by-products to obtain a filtrate;

[0040] (3) After the filtrate obtained in step (2) is rotary evaporated, the product obtained is PCETP according to the weight ratio of ethyl acetate and n-hexane 30:70 through a silica gel column;

Embodiment 3

[0042] The pyrene-functionalized RAFT reagent is used to illustrate the process of synthesizing pyrene-functionalized PSS through photoinitiated polymerization. The specific process includes the following steps:

[0043] (1) 23.9 mg of RAFT reagent (pyrene-functionalized 4-cyano-4-ethyltrithiopentanoic acid, PCETP), 2.06 g of a negatively charged monomer under neutral pH conditions (p-styrenesulfonic acid Sodium) and 1.5mg terpyridine ruthenium are dissolved in 50mL volumetric flask with 3.5mL water and 3.5mL dioxane to obtain reagent;

[0044] (2) feed nitrogen into the volumetric flask equipped with reagent in step (1) to remove oxygen for 30 minutes;

[0045] (3) irradiate and stir the volumetric flask after deoxygenation in step (2) under a 165W blue light for 24h;

[0046] (4) dialyze the product obtained in step (3) in ultrapure water for 3 days, then put it into a vacuum box and dry it to obtain the polymer PSS;

[0047] (5) The PSS synthesized by the above-mentioned ...

Embodiment 4

[0049] PSS1 is dissolved in water to obtain a 5mM PSS1 aqueous solution. The prepared PSS1 aqueous solution is mixed with a cation exchange resin (such as Nafion) at a volume ratio of 1:1, and then directly dripped onto the electrode surface and dried for 60 seconds by infrared to obtain a solid-state electrochemical solution. Luminescence sensor;

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Abstract

The invention belongs to the field of photo-initiation reversible addition fragmentation chain transfer (RAFT) polymerization and electrochemical luminescence sensor preparation, and relates to a method for modifying an electrode by using sodium polystyrenesulfonate (PSS) obtained through terpyridyl ruthenium [Ru(bpy)3<2+>] photo-initiation RAT polymerization together with a residual photoinitiator [Ru(bpy)3<2+>], so as to prepare a solid electrochemical luminescence sensor. The method comprises the following steps: preparing PSS by using functionalized cyan-4-ethyl trithioic valeric acid, by using negative charges of PSS and positive charges of a terpyridyl ruthenium initiator, adsorbing [Ru(bpy)3<2+>] by a final polymer product through electrostatic interaction, mixing the prepared PSS with cation exchange resin in a certain ratio, coating the surface of the electrode so as to prepare the solid electrochemical luminescence sensor, or directly soaking an electrode with a surface of a graphene plane into an aqueous solution of PSS for 12-48 hours, through pi-pi overlapping function of a pyrene functional group and the graphene surface, fixing the polymer PSS adsorbed with terpyridyl on the surface of the electrode so as to prepare the solid electrochemical luminescence sensor, and blow-drying with nitrogen.

Description

Technical field: [0001] The invention belongs to the field of light-induced reversible addition-fragmentation chain transfer (RAFT) polymerization and preparation of electrochemiluminescent sensors, and relates to a method for preparing chemical sensors, in particular to a method using ruthenium terpyridine [Ru(bpy) 3 2+ ] Photoinitiated RAFT polymerization obtained polystyrene sulfonate sodium (PSS) and residual photoinitiator [Ru(bpy) 3 2+ ] co-modified electrodes to prepare solid-state electrochemiluminescent sensors. Background technique: [0002] At present, due to the mild reaction conditions of photoinitiation and the ability to modify high-temperature volatile proteins such as enzymes and other biological materials, photoinitiation has attracted more and more attention and has been widely used in chemical industry and other fields. However, due to the narrow wavelength range that can initiate photopolymerization in the photoinitiation reaction, the low efficiency ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30G01N21/76
CPCG01N21/76G01N27/30
Inventor 许元红刘敬权陈涛
Owner QINGDAO UNIV
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