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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 preparation of solid phase extraction column, to achieve the effect of reducing matrix effect, high enrichment multiple and high enrichment efficiency

Inactive Publication Date: 2012-07-18
NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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  • Abstract
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  • 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

Method used

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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 estrogen molecular sealing column of estrogen molecules of the invention, including the following steps:

[0013] 1. Mix 100 ~ 500 mg phenol environment estrogen molecular marks with 5 ~ 20 mL pure organic solvents. After oscillation of 5 ~ 30 min, ultrasonic 5 ~ 30 minutes to mixingAfter the small column is extracted, after the loading is uniform, the two ends are blocked with a sieve plate.

[0014] Phenol environment estrogen molecular seal polymer is preferably powder -like.

[0015] Phenol environment estrogen molecular marks polymer can be prepared through the following steps:

[0016] (1) Preparation of high magnetic content single -decentralized tetraonic oxide / polymer composite microspheres: use chemical co -precipitation legal system to obtain nano -tanning three -iron particles, and use oleic acid for surface modification, and then use suspended polymerization to prepare legal preparation legal preparationGet high magnetic single -di...

Embodiment 1

[0028] Preparation of phenol environment estrogen molecular seal sealing columns:

[0029] (1) Mix the 100mg phenol environment estrogen molecular seal with 10ml pure organic solvents. After oscillation for 10 minutes, the ultrasound is 10min to mix uniformly, and move to the solid pillar of the material of polypropylene and other materials.Cover;

[0030] (2) Mix the 500mg traditional solid -phase extraction fillers with 10ml pure organic solvents. After oscillation for 10 minutes, the ultrasound is 10min to mix evenly.Use 10ml acidic organic solvents upper column to wash, and then wash with a 10ml pure organic solvent upper column to remove acidic substances;

[0031] (3) Step (2) The obtained solid phase extraction is removed with an inert gas to remove the residual organic solvents. The vacuum drying at 30 ° C for 12 hours, and the phenolic environmental estrogen molecular seal solid phase extraction column is obtained.

[0032] Performance evaluation of phenol environment est...

Embodiment 9

[0047] Example 9: Preparation of estrogen molecular marks polymer for phenolic environment

[0048] 1. Take 5.56G FESO respectively 4 ? 7h 2 O and 10.58G FeCl 3 ? 6h 2 O, dissolved in 200.0ml ultra -pure water, dispersed by ultrasound for 5.0 minutes, heated heating to 60 ° C, the stirring speed was 300 rpm, and the excess ammonia water was added to the pH of 11.0, the constant temperature and constant speed response was 1.0 hours, the magnetic separation, the use of the magnetic separation, the use of the magnetic separation, the use of the magnetic separation, the use of the magnetic separation, the use of the magnetic separation, the use of the magnetic separation, the use of the magnetic separation.Ultra-pure water and ethanol were washed several times to pH from 6-8, 60 ° C vacuum drying for 12 hours, and nano oxide triangular particles were made.

[0049] 2. Weigh the nano -four iron oxide particles prepared by Step 2.0 G, and add it to the 200.0ml ethanol solution. The ultr...

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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 involves a preparation method of solid -phase extraction column, especially the preparation method of a phenolic environmental estrogen molecular seal sealing column. Background technique [0002] Phenol environment estrogen as an additive for preparing epoxy resin and polycarbonate plastic. Entering the organism can cause endocrine disorders, endangers the germ function of the organism or cause malignant tumors, and increase hormone -related cancer.Environmental toxicity has attracted widespread attention from domestic and foreign researchers.The latest research shows that 0.1 μg / L or even lower -dimensional phenolic environmental estrogen can cause the biological effects of experimental animals, interfere with the secretion of endogenous hormones in the organism, and its low -dose effects have become the current phenol environment estrogenAn important direction of research.In view of this, the research on the enrichment of estrogen and detec...

Claims

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Application Information

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Patent Type & Authority Applications(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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