Preparation method of solid phase extraction column of molecular imprinted of phenolic environmental estrogens

A technology of environmental estrogen and solid phase extraction column, which is applied in the field of solid phase extraction column preparation, to achieve the effects of reducing matrix effect, high enrichment multiple, and strong selectivity

Inactive Publication Date: 2014-04-16
NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no report on the preparation method of molecularly imprinted solid-phase extraction column for phenolic environmental estrogen

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  • Preparation method of solid phase extraction column of molecular imprinted of phenolic environmental estrogens
  • Preparation method of solid phase extraction column of molecular imprinted of phenolic environmental estrogens
  • Preparation method of solid phase extraction column of molecular imprinted of phenolic environmental estrogens

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preparation example Construction

[0012] The preparation method of the phenolic environmental estrogen molecularly imprinted solid-phase extraction column of the present invention comprises the following steps:

[0013] 1. Mix 100-500 mg of phenolic environmental estrogen molecularly imprinted polymer with 5-20 mL of pure organic solvent, shake for 5-30 min, ultrasonicate for 5-30 min until the mixture is uniform, and transfer to a solid material such as polypropylene. In the phase extraction small column, after filling evenly, the two ends are respectively blocked with sieve plates.

[0014] The phenolic environmental estrogen molecularly imprinted polymer is preferably in powder form.

[0015] Phenolic environmental estrogen molecularly imprinted polymers can be prepared by the following steps:

[0016] (1) Preparation of monodisperse Fe3O4 / polymer composite microspheres with high magnetic content: Nano-Fe3O4 particles were prepared by chemical co-precipitation method, and the surface was modified with olei...

Embodiment 1

[0028] Preparation of phenolic environmental estrogen molecularly imprinted solid-phase extraction column:

[0029] (1) Mix 100mg of phenolic environmental estrogen molecularly imprinted polymer with 10mL of pure organic solvent, oscillate for 10 minutes, then sonicate for 10 minutes until the mixture is uniform, transfer to a solid-phase extraction column made of polypropylene or other materials, and use sieve plates at both ends blocking;

[0030] (2) Mix 500mg of traditional solid-phase extraction filler with 10mL of pure organic solvent, oscillate for 10 minutes and then sonicate for 10 minutes to mix evenly, then transfer to the solid-phase extraction column obtained in step (1), fill it evenly and seal the top with a sieve plate, Wash the column with 10mL of acidic organic solvent, and then wash with 10mL of pure organic solvent to remove acidic substances;

[0031] (3) The solid-phase extraction obtained in step (2) was purged with an inert gas to remove residual organ...

Embodiment 9

[0047] Example 9: Preparation of phenolic environmental estrogen molecularly imprinted polymers

[0048] 1. Weigh 5.56g FeSO 4 ?7H 2 O and 10.58 g FeCl 3 ?6H 2 O, dissolved in 200.0mL ultrapure water, ultrasonically dispersed for 5.0 minutes, heated to 60°C, stirring at 300 rpm, adding excess ammonia water to pH 11.0, reacting at constant temperature and speed for 1.0 hour, magnetic separation, successively Washing with ultra-pure water and ethanol for several times until the pH is 6-8, and drying in vacuum at 60°C for 12 hours to prepare nanometer ferric oxide particles.

[0049] 2. Weigh 2.0 g of the nano-iron ferric oxide particles prepared in step 1, and add it into 200.0 mL of ethanol solution, ultrasonically disperse for 5.0 minutes, and stir the reaction at a constant temperature of 60 ° C, the stirring speed is 300 rpm, 10 Add 20.0mL oleic acid dropwise at a constant rate within 1 minute, react for 1.0 hour, magnetically separate, wash with ethanol several times un...

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Abstract

The invention discloses a preparation method of a solid phase extraction column of molecular imprinted of phenolic environmental estrogens. The method comprises steps of: uniformly mixing 100-500mg of molecular imprinted polymer of phenolic environmental estrogens with 5-20mL of pure organic solvent, and uniformly mixing 100-500mg of traditional solid phase extraction packing with 5-20mL of pure organic solvent; orderly moving the mixtures into a hollow solid phase extraction column; plugging two ends of the solid phase extraction column with sieve plates; adding an acid organic solvent into the solid phase extraction column to wash after the solid phase extraction column being uniformly filled; flushing the filled solid phase extraction column with the pure organic solvent; purging the filled solid phase extraction column with inert gases to remove residual organic solvent; and drying to obtain the product. The preparation method disclosed by the invention is simple, and has particularity matching with the molecular imprinted polymer of phenolic environmental estrogens; and the prepared solid phase extraction column performs high selectivity and high recovery rate to the phenolic environmental estrogens, and is capable of obviously reducing the matrix effects.

Description

technical field [0001] The invention relates to a preparation method of a solid-phase extraction column, in particular to a preparation method of a phenolic environmental estrogen molecularly imprinted solid-phase extraction column. Background technique [0002] Phenolic environmental estrogens are used as additives for the preparation of epoxy resins and polycarbonate plastics. When they enter the organism, they can cause endocrine disorders, endanger the reproductive function of organisms or cause malignant tumors, and increase the incidence of hormone-related cancers. The biological estrogen effect And environmental toxicity has aroused widespread concern of researchers at home and abroad. The latest research shows that 0.1μg / L or even lower levels of phenolic environmental estrogen can cause biological effects in experimental animals and interfere with the secretion of endogenous hormones in organisms. an important direction of research. In view of this, the research o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/22
Inventor 赵永纲金米聪陈晓红
Owner NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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