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Application of rhodamine thiospirolactone in detection of mercury ions by up-conversion fluorescence analysis method

A technology for fluorescence analysis and mercury ions, which is applied in rhodamine thiospirolide (RhS) probes and high-concentration mercury ion detection applications, and can solve problems such as limiting the application of Stokes fluorescence recognition

Pending Publication Date: 2022-07-15
SUZHOU UNIV OF SCI & TECH
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  • Summary
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  • Description
  • Claims
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Problems solved by technology

However, the fluorescence detection method is only suitable for the detection of low-concentration mercury ions, because the conventional fluorescence method relies on the Stokes fluorescence technique
It is well known that Stokes fluorescence detection can only detect ions at very low concentrations (usually <10μM) due to its concentration quenching phenomenon (CIQ), which limits the application of Stokes fluorescence detection in high concentration range detection

Method used

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  • Application of rhodamine thiospirolactone in detection of mercury ions by up-conversion fluorescence analysis method
  • Application of rhodamine thiospirolactone in detection of mercury ions by up-conversion fluorescence analysis method
  • Application of rhodamine thiospirolactone in detection of mercury ions by up-conversion fluorescence analysis method

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Experimental program
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Effect test

Embodiment 1

[0030] Example 1 Preparation of Rhodamine Thiaspirolactone (RhS)

[0031] Rhodamine B (1 g, 2.6 mmol), phosphorus oxychloride (8 mL) and 20 mL of dichloroethane were added to a 50 mL three-necked flask; the reaction was refluxed at 90 °C for 12 h, and the reaction process was followed by spotting, and the developing solvent was Dichloromethane: petroleum ether (1 / 1, v / v), stop the reaction, cool to room temperature; dichloroethane and phosphorus oxychloride are distilled off under reduced pressure to obtain a khaki solid intermediate product (rhodamine acid chloride). In the case of no purification, the above intermediate product was directly dissolved in anhydrous tetrahydrofuran, and thiourea (10 mM, 760 mg) was added; under nitrogen atmosphere, the reaction was carried out at room temperature for 12 h; the reaction process was followed by spot plate, and the developing solvent was dichloride Methane: Petroleum ether (1 / 1, v / v). The reaction was stopped, cooled to room temp...

Embodiment 2

[0033] Preparation of probe (RhS) mother solution: Dissolve a certain amount of probe RhS in dimethyl sulfoxide (DMSO), mix with an equal volume of trimethylolamine methane / hydrochloric acid buffer aqueous solution (pH=7), and prepare A stock solution with a concentration of 2.0 mM was obtained and stored in the dark.

[0034] Preparation of probe (RhS) detection solution: take a certain amount of RhS mother solution and dilute it with different volumes of DMSO to obtain two RhS detection solutions of different concentrations: when used for conventional Stokes fluorescence detection, the RhS detection solution has The concentration is 10 μM; when used for OPA-UC detection, the concentration of RhS detection solution is 0.5 mM.

[0035] Preparation of metal ion solution to be tested: select 16 kinds of metal ions (respectively: Hg 2+ , Pb 2+ , Cd 2+ , Zn 2+ , Cu 2+ , Fe 2+ , Fe 3+ , Co 2+ , Ni 2+ , Mn 2+ , Mg 2+ , Ca 2+ , Na + , K + , Li + , NH 4 + ), and prepa...

Embodiment 3

[0036] Example 3 Probe RhS vs Hg 2+ selective response

[0037] Add 16 kinds (respectively: Hg 2+ , Pb 2+ , Cd 2+ , Zn 2+ , Cu 2 + , Fe 2+ , Fe 3+ , Co 2+ , Ni 2+ , Mn 2+ , Mg 2+ , Ca 2+ , Na + , K + , Li + , NH 4 + ) metal ion aqueous solution (100 μM, final concentration), and the upconversion fluorescence spectrum (OPA-UC detection, excitation wavelength of 655 nm) was measured immediately. attached by image 3 It can be seen that only when Hg is added 2+ Afterwards, broad and strong up-conversion fluorescence appeared, with a peak at ~590 nm, and a very strong orange-yellow fluorescence could be seen from the RhS detection solution with the naked eye. On the contrary, after adding the other 15 metal ions, the OPA-UC spectrum of the RhS detection solution hardly changed, and the RhS detection solution could not be observed to emit fluorescence with the naked eye.

[0038] attached Figure 4 and attached Figure 5 It can be seen that due to the spiro r...

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Abstract

The invention discloses application of rhodamine sulfur spirolactone in detection of mercury ions by an up-conversion fluorescence analysis method, a sample containing the mercury ions and a rhodamine sulfur spirolactone solution are mixed to obtain a mixed solution, then the mixed solution is irradiated by a 655 nm excitation light source, and when the wavelength range of emitted light is 565-630 nm, it is indicated that the sample contains the mercury ions. The invention discloses a single photon absorption up-conversion (OPA-UC) detection technology which can be used for detecting high-concentration mercury ions (mM of millimole concentration magnitude). The limitation that only low-concentration mercury ions (micromolar concentration magnitude, mu M) can be detected by using a conventional fluorescence (namely Stokes fluorescence) detection technology is overcome. Compared with a conventional fluorescence detection method, the OPA-UC method has the advantage that the concentration detection of mercury ions can be improved by 2 orders of magnitude.

Description

technical field [0001] The invention belongs to the field of one-photon absorption upconversion (OPA-UC). In particular, it relates to a rhodamine thiospironolide (RhS) probe with enhanced response of aggregated OPA-UC upconversion and the application of the probe in high-concentration mercury ion detection. Background technique [0002] Mercury ion pollution has many hazards, especially high concentrations of mercury ions have a greater impact on the human body and the environment. At present, there are many methods for the determination of mercury ions, such as spectrophotometry, fluorescence method, electrochemical method and atomic absorption spectrometry. Among them, fluorescence analysis is favored due to its advantages of high sensitivity, short detection time and relatively simple operation. However, the fluorescence detection method is only suitable for the detection of low concentrations of mercury ions, because the conventional fluorescence method relies on the ...

Claims

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Application Information

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IPC IPC(8): G01N21/64C07D495/10C09K11/06
CPCG01N21/6402G01N21/6447C07D495/10C09K11/06G01N2201/06113C09K2211/1096
Inventor 王筱梅陈泉仑叶常青陈硕然梁作芹李琳
Owner SUZHOU UNIV OF SCI & TECH
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