Preparation method and application of amino-modified Fe3O4 microspheres

An amino-modified, fe3o4-nh2 technology, applied in separation methods, chemical instruments and methods, other chemical processes, etc., can solve the problems of carcinogenesis, accelerated cell apoptosis, etc., to reduce matrix interference, simple preparation method and low price. Effect

Inactive Publication Date: 2020-07-31
JILIN INST OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, OA will also accelerate the apoptosis process of cells, and long-term accumulation can cause cancer.

Method used

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  • Preparation method and application of amino-modified Fe3O4 microspheres
  • Preparation method and application of amino-modified Fe3O4 microspheres
  • Preparation method and application of amino-modified Fe3O4 microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 1.35 g of ferric chloride hexahydrate, 3.6 g of anhydrous sodium acetate, 1.0 g of polyethylene glycol, and 0.5 g of cysteamine hydrochloride, dissolve them in 30 mL of ethylene glycol, and stir at room temperature for 20 min. Transferred to a 50 mL synthesis kettle, reacted at 190 °C under sealed conditions for 8 h, cooled to room temperature, washed the obtained magnetic nanomaterials with deionized water several times, and placed them in a vacuum oven at 60 °C for 4 h to obtain a black solid Fe 3 o 4 -NH 2 .

[0029] Below, Fe is characterized by SEM, EDS, Malvern particle sizer 3 o 4 -NH 2 physical and chemical properties.

[0030] Depend on figure 1 It can be seen that Fe 3 o 4 -NH 2 It has a spherical structure with a particle size of ~200 nm.

[0031] Depend on figure 2 It can be seen that there is N element in the adsorbent, which proves that cysteamine hydrochloride is successfully modified on Fe 3 o 4 surface.

[0032] Depend on image 3...

Embodiment 2

[0034] Present embodiment utilizes the Fe that embodiment 1 prepares 3 o 4 -NH 2 The method for extracting OA in scallops comprises the following steps:

[0035] Refer to the treatment method of scallop meat in the SN / T2269-2009 standard to prepare scallop extract, take an appropriate amount of scallop extract, and prepare a mixed solution with extract: ultrapure water = 2:8 (V:V), take 10 mL Mix the solution and add 20 mg Fe 3 o 4 -NH 2 , vortex extraction, magnetic separation, discard the supernatant, add eluent for elution, vortex elution again, after magnetic separation, N 2 Blow dry, constant volume with mobile phase, centrifuge at 12000 r / min for 10 min, take supernatant and pass through 0.22 μm filter membrane, then use UPLC-MS to measure the concentration of OA.

Embodiment 3

[0037] To investigate the effect of different pH on the Fe 3 o 4 -NH 2 effect on extraction performance.

[0038] According to the method described in Example 2, investigate the influence of the pH of the system on the extraction efficiency of the target substance, and study the Fe in the sample solution whose pH of the adsorption system is 3, 5, 7, 9, 11 3 o 4 -NH 2 Extraction efficiency of OA. Such as Figure 4 As shown, the extraction efficiency reaches the highest when pH=7.

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Abstract

The invention discloses a preparation method and application of amino modified Fe3O4 nano microspheres. By taking ferric trichloride hexahydrate, anhydrous sodium acetate, polyethylene glycol, cysteamine hydrochloride (CSH) and ethylene glycol as raw materials, the amino-modified Fe3O4 nano microspheres (Fe3O4-NH2) are prepared. Okadaic acid in scallops is extracted by using the Fe3O4-NH2 as an adsorbent. Extraction conditions of the Fe3O4-NH2 on okadaic acid are optimized; and when the pH value is 7, the mass of the adsorbent is 20 mg, the vortex adsorption time is 20 min, the eluent is a mixture of ammonia water and methanol in a ratio of 10%: 90%, and the volume of the eluent is 4 mL, the extraction efficiency of the Fe3O4-NH2 on the okadaic acid in shellfish is optimal.

Description

technical field [0001] The invention belongs to the field of inorganic-organic composite materials and technologies, and in particular relates to the preparation of a composite material, which can be used to extract okadaic acid in shellfish. Background technique [0002] Okadaic acid (OA) is a diarrheal shellfish toxin with good fat solubility. It is easy to accumulate in the body after being ingested by shellfish and other organisms, and it is transmitted to humans through the food chain, thereby causing poisoning reactions in the human body. In addition, OA will accelerate the apoptosis process of cells, and long-term accumulation can cause cancer. Therefore, the detection of OA in shellfish products is of great significance. [0003] Due to the complex matrix composition of shellfish samples, it is necessary to selectively enrich the OA in the sample before analyzing the OA through the instrument to exclude matrix interference. In recent years, on the basis of solid-ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/06B01J20/28B01J20/30B01D15/08B01D15/42
CPCB01J20/06B01J20/28009B01J20/28021B01D15/08B01D15/426
Inventor 连丽丽姜鑫浩娄大伟刘一民
Owner JILIN INST OF CHEM TECH
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