Nuclear magnetic resonance sensor for detecting melamine based on magnetic nanoparticles, and preparation method and application thereof

A technology of magnetic nanoparticles and melamine, applied in nuclear magnetic resonance analysis, nuclear magnetic resonance/magnetic resonance imaging contrast agents, etc., can solve problems such as urine can not be successfully discharged, renal tubular obstruction, renal failure, etc., and the preparation method is simple Safety, economy of raw materials, effect of enriching the research field

Inactive Publication Date: 2014-07-16
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the human body cannot convert these two substances, melamine and cyanuric acid are finally transported by the blood to the kidneys, where the two substances meet, and through the interaction of hydrogen bonds, a water-insoluble macromolecular co

Method used

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  • Nuclear magnetic resonance sensor for detecting melamine based on magnetic nanoparticles, and preparation method and application thereof
  • Nuclear magnetic resonance sensor for detecting melamine based on magnetic nanoparticles, and preparation method and application thereof
  • Nuclear magnetic resonance sensor for detecting melamine based on magnetic nanoparticles, and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0031] (1) Add 5.0g of cyanuric acid to 150mL of dry DMF, then add 1.15mL of DBU, 1.2mL of benzyl bromoacetate, stir at room temperature for 1h under Ar atmosphere, then heat to 70°C and keep for more than 12h, After the reaction was finished, cool to room temperature, remove DMF by distillation under reduced pressure, the obtained solid was washed and filtered with THF, the obtained filtrate was concentrated, washed with cold water, filtered and dried, and the obtained solid was analyzed by column chromatography (SiO 2 , CH 2 Cl 2 / MeOH, 24:1) separation and purification to obtain white solid benzyl ester.

[0032] (2) Dissolve 477mg NaOH in 15mL H 2 O, mix well, add 661mg benzyl ester, stir overnight at room temperature, after the reaction, acidify with 36wt% HCl, pH = 1, remove H by distillation under reduced pressure 2 O, the obtained substance was extracted several times by THF filtration, and the filtrate was concentrated to obtain a white solid specific receptor unit...

Embodiment 2

[0035] Take 20mL of octadecene with a measuring cylinder, 0.2mL of oleylamine with a pipette, and 0.1g of HDA·HCl with an analytical balance, add them into a three-necked flask, mix well, stir magnetically and remove the air, and the time is controlled at about 1h. The temperature was raised to 120°C and kept for 30 minutes. heated to 180°C with N 2 Gas protection, rapid injection of 0.7mL Fe(CO) 5 , maintaining the stirring speed at maximum. After keeping at 180°C for 20 minutes, inject oleic acid (0.3 mL, 1 mmol) and keep it for 10 minutes. Remove heat source, cool to room temperature, and expose to air. Centrifuge (12000rpm, 10min) until washed. Obtained Fe / Fe 3 o 4 Nanoparticles are dispersed in n-hexane.

[0036] The TEM figure of the magnetic nanoparticles prepared in this embodiment is as follows figure 2 shown; DLS as image 3 Shown; X-ray diffraction pattern as Figure 4 Shown; Infrared spectrum as Figure 5 shown.

Embodiment 3

[0038] (1) Analytical balance Weigh the acceptor unit (m=16.84mg, M=187.11g / mol, n=0.09mmol) and dissolve it in 5mL of pyridine, add 25mg of N-hydroxysuccinimide, and react for 1h to obtain solution A ; Dissolve polyethylene glycol monocarboxylic acid (m=60mg, M=2000g / mol, n=0.03mmol) in 5mL of pyridine with an analytical balance, add 10mg of N-hydroxysuccinimide, and react for 1h to obtain solution B .

[0039] (2) Analytical balance weighs Dopa-HCl (m=15.2mg, M=189.68g / mol, n=0.08mmol), 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride Dissolve 25 mg of salt in 1 mL of chloroform, and disperse evenly with ultrasonic waves to obtain solution A'; weigh Dopa-HCl (m=4 mg, M=189.68 g / mol, n=0.02 mmol), 1-ethyl-(3 - 10 mg of dimethylaminopropyl) carbodiimide hydrochloride was dissolved in 1 mL of chloroform, and ultrasonically dispersed to obtain solution B'; solution A' was added to solution A, and solution B' was added to solution B.

[0040] (3) Stir magnetically for...

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Abstract

The invention discloses a nuclear magnetic resonance sensor for detecting melamine based on magnetic nanoparticles. The nuclear magnetic resonance sensor is a Fe/Fe3O4 magnetic nanoparticle containing an acceptor unit which is capable of specific recognition of melamine and having water-solubility, superparamagnetism, uniform particle size distribution and a particle size of about 10 to 20 nm. A preparation method for the sensor comprises the following steps: preparation of a Fe/Fe3O4 magnetic nanoparticle through high temperature pyrolysis; preparation of Dopa-PEG and Dopa-acceptor unit by using N-hydroxy succinimide and 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride; and preparation of a target nanoparticle for preparation of the nuclear magnetic resonance sensor used for detecting melamine in virtue of coordination of oxygen and connection of the nanoparticle. The preparation method provided by the invention has the advantages of easiness, safety, economy and easy availability of raw materials and good process controllability. According to the invention, a novel prospect--a nanometer magnetic resonance sensor is provided for application of a nanometer magnetic resonance contrast agent material, and the research area of nano-materials is broadened.

Description

technical field [0001] The invention relates to the field of nuclear magnetic resonance sensing, in particular to a nuclear magnetic resonance sensor for detecting melamine based on magnetic nanoparticles, a preparation method and application thereof. Background technique [0002] A sensor is a device that detects or measures a physical property and records, displays or otherwise responds to it. Sensors can be divided into three categories, namely ① physical sensors, used to measure distance, mass, temperature, pressure, etc.; ② chemical sensors, which use chemical or physical responses to determine chemical substances; Detect chemicals. All of these devices must be connected to some kind of sensing device so that the response that occurs can be detected. The components mainly include: analytical mass, identification unit, conductor, and measuring device. [0003] Because ① MRI (magnetic resonance imaging, or magnetic imaging) has excellent resolution of soft tissues. Th...

Claims

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Application Information

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IPC IPC(8): A61K49/08G01N24/08
Inventor 杨仕平沈金超周治国孙亚楠张钖杨艳
Owner SHANGHAI NORMAL UNIVERSITY
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