Cyclodextrin-europium/lanthanum molybdate hybrid microsphere, preparation method thereof and application of cyclodextrin-europium/lanthanum molybdate hybrid microsphere in fluorescence detection of phosphorus-containing compound

A hybrid microsphere and fluorescence detector technology, applied in the field of fluorescence sensors, can solve the problems of limited application potential, and achieve the effects of improving application potential, excellent result accuracy, and strong functionality

Active Publication Date: 2021-11-02
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Cyclodextrin-europium/lanthanum molybdate hybrid microsphere, preparation method thereof and application of cyclodextrin-europium/lanthanum molybdate hybrid microsphere in fluorescence detection of phosphorus-containing compound
  • Cyclodextrin-europium/lanthanum molybdate hybrid microsphere, preparation method thereof and application of cyclodextrin-europium/lanthanum molybdate hybrid microsphere in fluorescence detection of phosphorus-containing compound
  • Cyclodextrin-europium/lanthanum molybdate hybrid microsphere, preparation method thereof and application of cyclodextrin-europium/lanthanum molybdate hybrid microsphere in fluorescence detection of phosphorus-containing compound

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preparation example Construction

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

[0051] 1) Mix β-cyclodextrin with a molar ratio of 1:(1-4) and sodium periodate in an aqueous solution, and stir and react at 30-50°C for 3-5 hours in the dark, and after nanofiltration, mix with excess The ethanol is stirred and mixed until the precipitate is separated out, and then filtered, washed and freeze-dried in sequence to obtain the aldehyde cyclodextrin;

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

[0053] 3) Add the crosslinking agent 4-amino-6-hydroxy-2-mercaptopyrimidine and the cosolvent DMF to the molybdenum-modified aldehyde cyclodextrin precursor liquid, and stir and react at 60-80°C for 10-30min to obtain Molybdenum-modified aldehyde-based cyclodextrin suspension; wherein, the molar rat...

Embodiment 1

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

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

[0058] 2) 62 mg of ammonium molybdate and 114 mg of aldehyde cyclodextrin (molar ratio 1:2) were dissolved in 20 mL of water to obtain a molybdenum-modified aldehyde 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...

Embodiment 2

[0065] In this example, the hybrid microspheres based on cyclodextrin-europium molybdate / lanthanum prepared in Example 1 are used as a fluorescent 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 dispersion of hybrid microspheres with a concentration of 0.25 mg / mL, which is used as a fluorescence detector;

[0067] Prepare sodium hydrogen phosphate standard solutions 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 when the excitation wavelength is 280nm, the results are as follows image 3 Shown, after adding hydrogen phosphate ion, the fluorescence emission peak at 598nm place strengthens, and the emissi...

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Abstract

The invention relates to a cyclodextrin-europium / lanthanum molybdate hybrid microsphere, a preparation method thereof and application of the cyclodextrin-europium / lanthanum molybdate hybrid microsphere in fluorescence detection of a phosphorus-containing compound. The preparation method comprises the steps of firstly, preparing a mixed solution containing a molybdenum source and aldehyde cyclodextrin; adding a cross-linking agent and a cosolvent into the mixed solution, and stirring for reaction to obtain a molybdenum modified aldehyde cyclodextrin suspension; and adding a lanthanum source and a europium source into the molybdenum modified aldehyde cyclodextrin suspension, continuously stirring for reaction, and purifying to obtain the cyclodextrin-europium molybdate / lanthanum hybrid microsphere. The prepared hybrid microsphere can be used as a fluorescence detector for qualitative or quantitative detection of phosphate ions, nitrobenzene phosphate or dinitrobenzene phosphate. Compared with the prior art, the advantages of simplicity in preparation, stable signal, high sensitivity, high selectivity, high interference resistance and the like are achieved, and meanwhile, the inorganic phosphate ions and the nitrobenzene phosphate are distinguished and detected through different fluorescent signal response modes.

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. As an essential nutrient for aquatic organisms and an indicator of water pollution, phosphate is a water quality indicator strictly controlled by various discharge standards. Organophosphates are an important class of bulk chemicals widely used as plasticizers and anti-oxidative plastic additives. They inevitably accumulate in the human body through various pathways, causing carcinogenicity, teratogenicity, neurotoxicity, and endocrine disruption. and adverse health consequences for future generations. Considering the different ecological and biological toxicity and rela...

Claims

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Application Information

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Patent Type & Authority Applications(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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