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A method for efficiently extracting endocrine disruptors in samples

A technology for endocrine disruptors and samples, applied in material separation, analysis materials, measurement devices, etc., can solve the problems of low extraction efficiency, large amount of organic solvent, and complicated steps in pretreatment technology, achieve high recovery rate, reduce organic solvents, etc. The amount of use, the effect of efficient extraction

Inactive Publication Date: 2011-12-21
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012]Technical problem: the purpose of the present invention is to overcome the defects of existing pretreatment technology such as low extraction efficiency, large amount of organic solvent, cumbersome steps, time-consuming, etc., and propose a method based on A New Method for Extraction and Concentration of Target Substances in Samples—Endocrine Disruptors by Nylon Nanofiber Membrane

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Sample: environmental water sample

[0028] Target substances: dimethyl phthalate, diethyl phthalate, butyl benzyl phthalate, dibutyl phthalate, di(2-ethyl)hexyl phthalate, Di-n-octyl phthalate.

[0029] Nylon 6 was used as raw material, formic acid was used as solvent, and the mass concentration of nylon 6 was 25%. The electrospinning solution was obtained by magnetic stirring, and the nanofiber film was electrospun into a film with a thickness of 30 μm. The surface of the fiber is smooth and the diameter is 200~500nm.

[0030] Weigh 1.5mg of nanofiber membrane and put it into the membrane disk solid phase extraction apparatus, activate and wash with acetone→water→acetone→water (200μl each), adjust the pH of 50mL environmental water sample to 7.0 (the pKa value of the target substance is 9.0~9.7) , add sodium chloride to increase the ionic strength by 0.02mol / L, pass through the nanofiber membrane continuously at a speed of 4 mL / min, elute the target substance enrich...

Embodiment 2

[0032] Sample: Milk

[0033] Target substances: dimethyl phthalate, diethyl phthalate, butyl benzyl phthalate, dibutyl phthalate, di(2-ethyl)hexyl phthalate, Di-n-octyl phthalate.

[0034] Nylon 6 was used as raw material, formic acid was used as solvent, and the mass concentration of nylon 6 was 44%. The electrospinning solution was obtained by magnetic stirring, and the nanofiber film was electrospun into a film with a thickness of 60 μm. The surface of the fiber is smooth and the diameter is 300~600nm.

[0035] Weigh 2.5 mg of nanofiber membrane and load it into a membrane-disk solid-phase extraction apparatus, activate and wash with water→dichloromethane→water→dichloromethane→water (200 μl each), and adjust the pH to 6.5 ( The pKa value of the target substance is 9.0~9.7), add sodium acetate to increase the ionic strength by 0.05mol / L, pass through the nanofiber membrane continuously at a speed of 4 mL / min, and 100 μL acetone elutes the target substance enriched on the n...

Embodiment 3

[0037] Sample: bottled mineral water

[0038] Target substance: Bisphenol A

[0039] Nylon 66 is used as raw material, formic acid / m-cresol (v / v=3 / 2) is used as solvent, the mass concentration of nylon 66 is 30%, the electrospinning solution is obtained by heating and magnetic stirring, and the nanofiber film is electrospun into a film thickness of 50 μm. The surface of the fiber is smooth and the diameter is 300~600nm.

[0040] Weigh 1.5 mg of nanofiber membrane and put it into a membrane disc solid phase extraction apparatus, activate and wash with methanol→water→methanol→water (100 μl each), adjust the pH of 10mL sample to 7.0 (the pKa value of the target substance is 9.5), and use 3 mL / min speed flow-stop-flow-stop-flow, passing through the nanofiber membrane intermittently, 300 μL methanol elutes the target substance enriched on the nanofiber membrane, and takes 20 μL of the eluate for high performance liquid chromatography-UV absorption detection. The detection limi...

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Abstract

In the method for efficiently extracting endocrine disruptors in a sample of the present invention, the sample to be tested is preliminarily treated by filtering, grinding, homogenizing, ultrasonication, protein precipitation, protein hydrolysis or degreasing to make a sample solution of an aqueous matrix; adjust the pH value of the sample solution, Or add inorganic salts or organic salts to increase the ionic strength of the sample solution to reduce the distribution coefficient of endocrine disruptors in the water phase; use the membrane disc solid phase extraction device to make the sample solution flow continuously or "flow-stop-flow" intermittent Through the activated nylon nanofiber membrane, the endocrine disruptors in the sample are retained by the nylon nanofiber to achieve extraction. The invention synergizes the advantages of solid-phase membrane extraction and nano-adsorption media, and can realize efficient extraction of internally distributed interfering substances in various actual samples with only a few milligrams of nylon nanofiber membrane and hundreds of microliters of elution solvent , The extraction and enrichment process of separation, adsorption, concentration and elution can be completed within a few minutes to ten minutes.

Description

technical field [0001] The invention provides a method for efficiently extracting and enriching endocrine disruptors, which are targets in a sample to be tested, based on a nylon nanofiber membrane, and belongs to the technical field of sample pretreatment in analytical chemistry. Background technique [0002] The pollution of endocrine disrupting chemicals (EDCs) has become a major global problem. EDCs exist widely in nature and seriously interfere with natural hormones to maintain biological homeostasis and regulate development. The United States Environmental Protection Agency (USEPA) announced in August 1998 that 67 types (categories) of EDCs that endanger human body and organisms were screened out from 86,000 commercial products and chemicals. The assessment of pollution and exposure levels of EDCs is related to human life and health, and the core issue is to establish efficient, sensitive and accurate detection methods for endocrine disruptors in various environmental...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08
Inventor 许茜顾忠泽
Owner SOUTHEAST UNIV
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