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Fluorescence enhancement type hypochlorite detection method and application

A technology for detecting hypochlorous acid and fluorescence enhancement, which is applied in the fields of fluorescence/phosphorescence, measuring devices, and material analysis through optical means. It can solve the problems of difficult detection of hypochlorite ions and low detection sensitivity, and increase the scope of practical applications. , Strong anti-interference ability and high anti-interference effect

Active Publication Date: 2018-11-27
河南省联检药物分析有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention proposes a fluorescence-enhanced method and application for detecting hypochlorite, which solves the technical problems of difficult detection and low detection sensitivity of hypochlorite ions in tap water and food

Method used

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  • Fluorescence enhancement type hypochlorite detection method and application
  • Fluorescence enhancement type hypochlorite detection method and application
  • Fluorescence enhancement type hypochlorite detection method and application

Examples

Experimental program
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Effect test

preparation example Construction

[0036] 1. Preparation of fluorescent probe SRh

[0037] 1. Preparation of RhB-SH

[0038] In a 100 mL round bottom flask, dissolve 2.18 g (4.5 mmol) of rhodamine B in 30 mL of anhydrous 1,2-dichloroethane, and add 1.5 mL (16.4 mmol) of phosphorus oxychloride dropwise under ice-cooling conditions , react in ice bath (0°C) for 1 hour, change to reflux reaction at 85°C for 3 hours, remove the solvent under reduced pressure to obtain rhodamine acid chloride RhB-Cl; dissolve rhodamine acid chloride RhB-Cl in 30 mL of anhydrous acetonitrile, Add 0.51 g (4.5 mmol) cysteamine hydrochloride in anhydrous acetonitrile solution (15 mL) dropwise under ice bath (0°C) condition, react in ice bath for 6 hours, warm the reaction system to room temperature, remove the solvent under reduced pressure, and use Ethyl acetate (35 mL) was redissolved, washed with pure water (40 mL×2) and saturated sodium chloride solution (40 mL×2), the organic phase was dried over anhydrous sodium sulfate, filtered...

Embodiment 1

[0046] Prepare a Tris buffer solution with a pH of 7.4 and a concentration of 10 mM, use the above buffer solution and ethanol to prepare a mixed solution A with a volume ratio of 7:3, and use ethanol to prepare a probe SRh solution with a concentration of 1 mM. The effect of probe SRh on hypochlorite (ClO - ) in the selectivity of mixed solution A. Such as figure 1 As shown, under the excitation condition at 525 nm, the single probe SRh (10 µM) has a weak fluorescence emission intensity at 585 nm in mixed solution A, when adding hypochlorite (ClO - ) (10 eq.), the fluorescence emission intensity at 585 nm was significantly enhanced, but when other substances (100 µM) were added, the fluorescence emission intensity of the solution system did not change significantly compared with that of the probe system alone.

[0047] The above experimental results show that the probe SRh is sensitive to hypochlorite (ClO - ) has better fluorescence-specific selectivity in mixed solution...

Embodiment 2

[0049] Prepare a Tris buffer solution with a pH of 7.4 and a concentration of 10 mM, use the above buffer solution and ethanol to prepare a mixed solution A with a volume ratio of 7:3, and use ethanol to prepare a probe SRh solution with a concentration of 1 mM. In 20 clean fluorescent cuvettes, add 3000 μL of mixed solution A and 30 μL of probe SRh ethanol solution, and then add 10 molar equivalents of ClO - and 10 molar equivalents of other analytes (Br - , Cl - , F - , I - , CO 3 2- , HCO 3 - , PO 4 3- , HPO 4 2- , H 2 PO 4 - ,HS - , NO 2 - , NO 3 - , MnO 4 - , SO 4 2- , H 2 o 2 , KO 2 , TBHP, Cys, GSH) were detected on a fluorescence spectrometer, and the histograms of the 585 nm fluorescence intensities corresponding to different analytes were drawn to obtain the fluorescence emission histograms (attached figure 2 ).

[0050] It has been proved by experiments that the probe SRh is sensitive to hypochlorite (ClO - ) in the mixed solution A is n...

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Abstract

The invention relates to a hypochlorite (ClO-) detection technology, in particular to a fluorescence enhancement type hypochlorite detection method and application. The method is used for closed-loopand open-loop detection of hypochlorite on the basis of a rhodamine derivative (SRh) containing double C=S bond structures. The detection method specifically includes the steps that SRh serves as a fluorescence detection reagent, the probe SRh is subjected to a desulfurization reaction by using the strong oxidizing property of the hypochlorite in a CH3CH2OH-Tris solution system, a five-membered ring in a probe structure releases strong fluorescence from a closed loop to an open loop, the fluorescence of the solution system is remarkably enhanced, and then the hypochlorite is detected. The detection method shows high sensitivity to the hypochlorite, the lowest detection limit is as low as 2.43*10<-9> mol / L, the detection process is simple and convenient, the anti-interference capability ishigh, the method is rapid and sensitive, and detection results are accurate.

Description

technical field [0001] The present invention relates to hypochlorite (ClO - ) detection technology, especially a fluorescence-enhanced method and application for detecting hypochlorite. Background technique [0002] Hypochlorite ion (ClO - ) is closely related to our daily life and is widely used in daily life, such as household disinfectant and bleach. However, excess hypochlorite solution can pose a health hazard to humans and animals. On the other hand, the hypochlorite ion (ClO - ) is an important reactive oxygen species in organisms, which has important physiological functions in organisms, participates in many physiological activities, and plays a key role in the immune system. Studies have shown that abnormal hypochlorite levels in organisms can cause various diseases, such as Parkinson's disease, Alzheimer's disease, multiple sclerosis and cancer. Therefore, the development of rapid, sensitive, and specific methods for the detection of hypochlorite ions is of gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
CPCG01N21/6428
Inventor 贾斌张迪李漫刘继红王允尹海燕曹成郑嘉马莹刘冬梅李淑芳
Owner 河南省联检药物分析有限公司