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Co-detection method for estrogen coalition in water environment

A detection method and combination technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of large matrix interference and difficult processing technology, and achieve low detection limit, simple operation, high sensitivity and accuracy Effect

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 traces of estrogen conjugates in the water environment, large matrix interference, and difficult pretreatment technology, so as to realize the analysis of water Four kinds of estrogen conjugates in environmental samples, estrone sulfate conjugate (Estrone-3-sulfate, E1-3S), 17β-estradiol sulfate conjugate (Estradiol-3-sulfate, E2-3S) and estrone Quantitative determination of glucuronide (Estrone-3-glucuronide, E1-3G) and 17β-estradiol glucuronide (E2-3G)

Method used

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  • Co-detection method for estrogen coalition in water environment
  • Co-detection method for estrogen coalition in water environment
  • Co-detection method for estrogen coalition in water environment

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Embodiment Construction

[0040] The technical scheme of the present invention will be further described below in conjunction with examples and drawings

[0041] (1) HLB column enrichment

[0042] Take 4L of water sample using GF / F glass fiber filter membrane to filter, and adjust the pH to 3 with 4mol / L hydrochloric acid; use a solid phase extraction device to activate Waters HLB solid phase extraction column (200mg, 6cc), the order of activation is :5mL chromatographic pure ethyl acetate, 5mL chromatographic pure methanol and 10mL ultrapure water, the flow rate is 1mL / min; the activated solid phase extraction column is used for solid phase extraction and enrichment of the mixed solution, and the flow rate is controlled to 3mL / min; After the extraction is finished, it is vacuum-dried for 5 minutes, and it is to be purified.

[0043] (2) NH2 column purification

[0044] Connect the Waters NH2 column (500mg, 6cc) activated with 5mL methanol to the bottom of the dry HLB column with a solid phase extraction colu...

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Abstract

The invention relates to a detecting technique for an endocrine disrupter in a water environment and especially relates to a co-detection method for an estrogen coalition, Estrone-3-sulfate, E1-3S, Estradiol-3-sulfate, E2-3S, Estradiol-3-glucuronide, E1-3G and17beta-Estradiol-3-glucuronide, E2-3G in a water sample by adopting a liquid chromatogram-tandem mass spectrum technique. The method comprises the steps of: enriching the E1-3S, E2-3S, E1-3G and E2-3G in a collected water sample by using a HLB (Hydrophile-Lipophile Balance) solid-phase extraction column; connecting an activated NH2 column under the HLB column and washing with carbinol; and lastly, eluting with 2% of ammonia water carbinol solution and analyzing by adopting the liquid chromatogram-tandem mass spectrum technique. The method has the advantages of environmental protection, easiness in operation, high recovery rate and quick analysis for the trace amount of estrogen coalition E1-3S, E2-3S, E1-3G and E2-3G in the watersample.

Description

Technical field [0001] The invention relates to the technical field of detection of organic pollutants in the water environment, in particular to the extraction, purification and instrument detection methods of trace natural estrogen conjugates in natural water samples. Background technique [0002] Natural estrogen (Estrone, E1), 17β-Estradiol (17β-Estradiol, E2), estriol (Estriol, E3) and synthetic estrogen estrogen ethinyl estradiol secreted by human or mammalian ovaries (17α-Ethinyl Estradiol, EE2) is the most potential endocrine disrupting compound (Endocrine Disrupting Compounds, EDCs) at the risk of feminization. The concentration of ng / L in the water environment will lead to feminization of fish. When estrogen is discharged, the hydroxyl group at the C3- or C7-position in the estrogen molecular structure is mostly replaced by sulfate or glucuronic acid, which turns into a combination structure without estrogen activity, but in water bodies or sewage treatment plants biolo...

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Application Information

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Patent Type & Authority Applications(China)
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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