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A cyclodextrin-europium molybdate/lanthanum hybrid microsphere and its preparation method and its application in the fluorescence detection of phosphorus-containing compounds

A technology of hybrid microspheres and fluorescence detectors, applied in the field of fluorescence sensors, can solve problems such as limited application potential, and achieve the effects of improving application potential, mild synthesis conditions, and simple preparation methods

Active Publication Date: 2022-07-05
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the practical application potential of the dual-emitting lanthanide europium metal-organic framework material in this patent as a fluorescent probe for phosphate ions is limited

Method used

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  • A cyclodextrin-europium molybdate/lanthanum hybrid microsphere and its preparation method and its application in the fluorescence detection of phosphorus-containing compounds
  • A cyclodextrin-europium molybdate/lanthanum hybrid microsphere and its preparation method and its application in the fluorescence detection of phosphorus-containing compounds
  • A cyclodextrin-europium molybdate/lanthanum hybrid microsphere and its preparation method and its application in the fluorescence detection of phosphorus-containing compounds

Examples

Experimental program
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preparation example Construction

[0050] A hybrid microsphere based on cyclodextrin-europium molybdate / lanthanum, the preparation method comprising the following steps:

[0051] 1) Mix β-cyclodextrin and sodium periodate with a molar ratio of 1:(1-4) in an aqueous solution, and stir the reaction at 30-50 ° C in the dark for 3-5 h, after nanofiltration, mix with excess Ethanol is stirred and mixed until the precipitation is precipitated, and then the aldehyde-based cyclodextrin is obtained after filtration, washing and freeze-drying in sequence;

[0052] 2) co-dissolving ammonium molybdate and aldehyde-based cyclodextrin in water at a molar ratio of 1:2 to obtain a molybdenum-modified aldehyde-based cyclodextrin precursor liquid;

[0053] 3) adding the cross-linking agent 4-amino-6-hydroxy-2-mercaptopyrimidine and the cosolvent DMF to the molybdenum-modified aldehyde-based cyclodextrin precursor liquid, and stirring and reacting at 60-80 ° C for 10-30 min to obtain Molybdenum-modified aldehyde-based cyclodextr...

Embodiment 1

[0056] A hybrid microsphere based on cyclodextrin-europium molybdate / lanthanum, the preparation method comprising the following steps:

[0057] 1) Add 15g β-cyclodextrin into 100mL deionized water, stir evenly, then add 6g sodium periodate, and stir for 4h at 40°C in the dark, then filter through a 220nm filter membrane, take the filtrate And mixed with excess absolute ethanol (800mL) to precipitate out, and then successively filtered, washed with ethanol / water (V / V=80 / 20) for many times, and freeze-dried to obtain good water solubility, high reactivity, and containing bisulfite. Aldehyde-based cyclodextrin with aldehyde structure;

[0058] 2) co-dissolving 62 mg of ammonium molybdate and 114 mg of aldehyde-based cyclodextrin (molar ratio 1:2) in 20 mL of water to obtain a molybdenum-modified aldehyde-based cyclodextrin precursor liquid;

[0059] 3) Add 56 mg of cross-linking agent 4-amino-6-hydroxy-2-mercaptopyrimidine (the molar ratio of cross-linking agent to aldehyde cycl...

Embodiment 2

[0065] In this example, the hybrid microsphere based on cyclodextrin-europium molybdate / lanthanum prepared in Example 1 is used as a fluorescence sensor to detect phosphate ions in water samples. The specific detection process is as follows:

[0066] 1) Draw a standard curve: Disperse the hybrid microspheres based on cyclodextrin-europium molybdate / lanthanum in deionized water to form a hybrid microsphere dispersion with a concentration of 0.25 mg / mL, which is used as a fluorescence detector;

[0067] Prepare standard solutions of sodium hydrogen phosphate with concentrations of 0, 0.1, 0.5, 1.0, 2.5, 5, 10, 25, 50, 75, and 100 μM respectively, and mix 1 mL of each with an equal volume of fluorescence detector, and then use a fluorescence spectrometer to measure The emission spectrum at the excitation wavelength of 280 nm, the results are as follows image 3 As shown, after adding hydrogen phosphate ion, the fluorescence emission peak at 598nm is enhanced, and the emission pea...

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Abstract

The invention relates to a cyclodextrin-europium molybdate / lanthanum hybrid microsphere and its preparation method and application in the fluorescence detection of phosphorus-containing compounds. The preparation method includes first preparing a mixed solution containing a molybdenum source and an aldehyde-based cyclodextrin ; Add the cross-linking agent and the cosolvent to the mixed solution, and stir the reaction to obtain the molybdenum-modified aldehyde-based cyclodextrin suspension; then add the lanthanum source and the europium source to the molybdenum-modified aldehyde-based cyclodextrin suspension cyclodextrin-europium molybdate / lanthanum hybrid microspheres are obtained after purification treatment; the prepared hybrid microspheres can be used as fluorescence detectors for phosphate ions, nitrophenyl phosphate or In the qualitative or quantitative detection of bisnitrophenyl phosphate. Compared with the prior art, the invention has the advantages of simple preparation, stable signal, high sensitivity, strong selectivity, strong anti-interference and the like. Differential detection of phosphate esters.

Description

technical field [0001] The invention belongs to the technical field of fluorescence sensors, and relates to a cyclodextrin-europium molybdate / lanthanum hybrid microsphere, a preparation method thereof, and an application in fluorescence detection of phosphorus-containing compounds. Background technique [0002] Phosphates and organophosphates play key roles in various environmental and biological processes. Phosphate, as an essential nutrient for aquatic organisms and an indicator of water pollution, is a water quality indicator strictly controlled by various discharge standards. Organophosphates are an important class of bulk chemicals, widely used as plasticizers, antioxidant plastic additives, they inevitably accumulate in the human body through various pathways, resulting in carcinogenicity, teratogenicity, neurotoxicity, endocrine disruption and adverse health consequences for offspring. Considering the different ecological and biological toxicity and related control ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/16C09K11/02C09K11/78G01N21/64
CPCC08B37/0015G01N21/643C09K11/025C09K11/7794G01N2021/6432Y02A20/20
Inventor 毛舜李秋菊
Owner TONGJI UNIV
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