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Method for jointly detecting estrogen, nonyl phenol, octylphenol and bisphenol A in complex substrate water sample

A complex matrix, nonylphenol technology, applied in the field of estrogen and nonylphenol, bisphenol A extraction, purification and instrument detection, octylphenol, can solve the problem of large matrix interference, difficult pretreatment technology, estrogen Low detection limit, high recovery rate and high sensitivity can be achieved

Inactive Publication Date: 2012-08-15
BEIJING NORMAL UNIVERSITY
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Problems solved by technology

[0005] The purpose of the present invention is to develop a high recovery, high sensitivity, accurate and rapid analysis technology for the problems of trace amounts of estrogen in complex matrix water samples, large matrix interference, and difficult pretreatment technology, so as to realize the detection of estrogen. Quantitative determination of ketones, 17β-estradiol, estriol, 17α-ethynylestradiol, nonylphenol, octylphenol and bisphenol A

Method used

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  • Method for jointly detecting estrogen, nonyl phenol, octylphenol and bisphenol A in complex substrate water sample
  • Method for jointly detecting estrogen, nonyl phenol, octylphenol and bisphenol A in complex substrate water sample
  • Method for jointly detecting estrogen, nonyl phenol, octylphenol and bisphenol A in complex substrate water sample

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Embodiment Construction

[0037] Below in conjunction with example and accompanying drawing, technical scheme of the present invention is described further

[0038] (1) HLB column enrichment

[0039]Get 0.5L certain sewage treatment plant water sample, adopt GF / F glass fiber filter membrane to filter, and be 3 with the hydrochloric acid adjustment pH of 4mol / L; Utilize the HLB solid-phase extraction column (200mg, 6cc ), the activation sequence is: 5mL chromatographically pure ethyl acetate, 5mL chromatographically pure methanol, and 10mL ultrapure water, with a flow rate of 1mL / min; 3mL / min; after the enrichment is completed, first rinse with 6mL of 40% methanol aqueous solution, and then rinse with 6mL of methanol / ammonia / water solution, the methanol / ammonia / water solution v / v / v=10 / 2 / 88; After washing, vacuum-dry for 10 min, then elute with 6 mL of methanol, and dry the eluent with liquid nitrogen.

[0040] (2)Florisil column purification

[0041] Redissolve the nitrogen-dried residue with 6 mL of...

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Abstract

The invention relates to a detecting technique of endocrine disrupters in water environment and particularly relates to a technique for quantitative analysis on oestrone, 17beta-estradiol, estriol, 17alpha-ethinyl estradiol, nonyl phenol, octylphenol and bisphenol A in a complex substrate water sample by adopting a liquid chromatogram-tandem mass spectrum combined technique. The method comprises the following steps: enriching a collected water sample by using a HLB (Hydrophile-Lipophile Balance) solid-phase extraction column and washing with carbinol; drying elution liquid nitrogen and purifying by using Florisil; and finally, analyzing by utilizing the liquid chromatogram-tandem mass spectrum combined technique. The method is environment-friendly, easy to operate and high in recovery rate. The method can quickly analyze the trace amount of oestrone, 17beta-estradiol, estriol, 17alpha-ethinyl estradiol, nonyl phenol, octylphenol and bisphenol A in the complex substrate water sample.

Description

technical field [0001] The invention relates to the technical field of detection of organic pollutants in water environment, in particular to the extraction, purification and instrument detection methods of estrogen, nonylphenol, octylphenol and bisphenol A in complex matrix water samples. Background technique [0002] In recent years, natural and synthetic estrogens estrone (Estrone, E1), 17β-estradiol (17β-Estradiol, E2), 17α-ethinyl estradiol (17α-Ethinyl Estradiol, EE2), and estrogen-like activity The substances nonylphenol (Nonylphenol, NP), octylphenol (Octylphenol, OP) and bisphenol A (BisphenolA, BPA), as typical endocrine disruptors in the environment, have attracted widespread attention in the academic community. Relevant investigations and studies have shown that estrogen at the ng / L concentration level in the water environment is sufficient to cause the feminization of aquatic organisms. The estrogen emitted by the urine and feces of humans and mammals, and the ...

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Application Information

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IPC IPC(8): G01N30/88
Inventor 史江红吴唯张晖陈庆彩刘晓薇薄婷贾彦舶
Owner BEIJING NORMAL UNIVERSITY
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