Preparation method and chemiluminescence analysis method of R6GHO

A chemiluminescence and hydrazide technology, which is applied in the field of chemiluminescence determination of nitrite, can solve the problems of low selectivity and limited measurement objects.

Inactive Publication Date: 2018-04-20
CHENGDU UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the chemiluminescent systems of these reagents can meas

Method used

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  • Preparation method and chemiluminescence analysis method of R6GHO
  • Preparation method and chemiluminescence analysis method of R6GHO
  • Preparation method and chemiluminescence analysis method of R6GHO

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) In a 100mL three-necked flask, add 2.40g of rhodamine 6G and 60mL of hot absolute ethanol, cool slightly after the rhodamine 6G is completely dissolved, then add 8mL of 80% hydrazine hydrate dropwise while stirring, and reflux in a hot water bath for 2 hours. After the reaction was completed, part of the solvent was removed by rotary evaporation, and an khaki solid was precipitated, filtered with suction, washed with a small amount of frozen water, and dried to obtain 2.0 g of khaki powder with a yield of 95.2%.

[0030] 2) Add 0.912g R6GH to a 100mL two-necked flask, and then add 35mL dichloromethane to completely dissolve R6GH, then cool with a cold water bath. Dissolve 0.1mL (slightly excess) of oxalyl chloride in 10mL of dichloromethane, and add it dropwise to the above-mentioned 100mL two-necked flask under vigorous stirring (Note: R6GH and glass instruments should be dried before use). After the addition, the stirred mixture was placed in a cold water bath for ...

specific Embodiment 2

[0032] Solution preparation:

[0033] 1) Preparation of rhodamine 6G hydrazide oxamide standard solution

[0034]Accurately weigh 0.2276g of rhodamine 6G hydrazide oxamide (R6GHO) with an analytical balance into a 50ml beaker, add 2ml of 2mol / L HCl solution, stir with a thin glass rod to completely dissolve R6GHO, then add an appropriate amount of deionized water, and then transfer to In a 250ml volumetric flask, wash the small beaker and thin glass rod, and transfer the washing solution into the above-mentioned volumetric flask together, and finally make it to volume. The concentration of the resulting R6GHO standard solution is 1.00 × 10 -3 mol / L.

[0035] 2) Preparation of sodium nitrite (NO 2- )standard solution

[0036] Use a pipette to accurately pipette 10.00ml of 10.0mmol / L sodium nitrite solution into a 100ml volumetric flask, set the volume to the mark, shake well and put it in a dark place to obtain 1.0mmol / L sodium nitrite (NO 2- ) stock solution.

[0037] R6...

Embodiment 3

[0045] Determination of NO in saliva by the chemiluminescence system of the present invention 2- content:

[0046] Sample Processing: Saliva samples were obtained from four volunteers who were asked to rinse their mouths before collecting the samples. The collected samples were first centrifuged at a speed of 12000r / min for 10min to remove the protein in the saliva, and then 1ml of the supernatant was taken in a 100ml volumetric flask for later use.

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Abstract

The invention relates to a preparation method and a chemiluminescence analysis method of R6GHO, and discloses a preparation method of rhodamine 6G hydrazide oxamide and a new method for determining the content of nitrites in a water phase by using the synthesized R6GHO. The R6GHO reacts with hydrogen peroxide and nitrite ions under an acidic condition to make a five-membered amide ring be opened and form azide, and the azide is converted into strong-fluorescence rhodamine 6G together with energy change. An R6GHO fluorescence probe makes up for some function defects of a single-molecule probe,and has the advantages of high sensitivity, high selectivity, high reliability, and facilitation of analysis and detection.

Description

technical field [0001] The invention belongs to the field of chemiluminescence analysis, and relates to a preparation process of R6GHO and a new method for chemiluminescence determination of nitrite based on the high selectivity of rhodamine 6G hydrazide oxalamide (R6GHO) to nitrite. Background technique [0002] Chemiluminescence is the phenomenon in which visible light is emitted during certain chemical reactions. Its luminescent mechanism is that certain molecules in the reaction system, such as reactants, intermediates or fluorescent substances, absorb the energy released by the reaction and transition from the ground state to the excited state, and then return from the excited state to the ground state, and at the same time radiate the energy as light released in the form of chemiluminescence. The earliest discovered chemiluminescent phenomenon occurs in organisms, such as fireflies, which is now called bioluminescence, which is named after the visible light emitted by...

Claims

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Application Information

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IPC IPC(8): G01N21/76
CPCG01N21/76
Inventor 孙永华金燕李崇瑛
Owner CHENGDU UNIVERSITY OF TECHNOLOGY
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