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Method for testing water deposits or estrogen coalitions in soil

A sediment and estrogen technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of difficult pretreatment technology and the existence of trace amounts of estrogen substances, and achieve fast extraction speed, high sensitivity and precision, Sensitive effect

Inactive Publication Date: 2012-01-25
BEIJING NORMAL UNIVERSITY
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Problems solved by technology

[0005] The purpose of the present invention is to solve the problems of complex sediment sample matrix, trace amount of estrogen substances in the sediment, and difficult pre-treatment technology, and intends to develop a high-recovery, high-sensitivity, accurate and fast analysis technology to realize the Quantitative determination of estrogen conjugates E1-3S, E2-3S and E1-3G, E2-3G in sediment samples

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  • Method for testing water deposits or estrogen coalitions in soil
  • Method for testing water deposits or estrogen coalitions in soil
  • Method for testing water deposits or estrogen coalitions in soil

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Embodiment Construction

[0037] The technical solutions of the present invention will be further described below in conjunction with examples and accompanying drawings.

[0038] (1) Sediment sample extraction

[0039] The collected sediment samples were first freeze-dried, crushed with a wooden stick and passed through a 60-mesh nylon sieve. Accurately weigh 5 g of the freeze-dried sample, and use 60 ml of acetonitrile: water = 9: 1 (v / v) as the extractant for rapid solvent extraction. For the fast solvent extraction method adopted, the selected temperature is 60°C, the pressure is 1500pis, and the static extraction is performed twice, 8 minutes each. Concentrate the extract to about 1ml with a rotary evaporator, transfer it to a 50ml centrifuge tube and dry it with nitrogen in a water bath at 37°C, then redissolve the residue with 1ml of methanol.

[0040] (2) Solid phase extraction (SPE) purification

[0041] The methanol-dissolved residue was first passed through an activated NH2 column (6cc, 50...

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Abstract

The invention provides a method for testing water deposits or estrogen coalitions in soil. Water deposits or four estrogen coalitions, namely E1-3S, E2-3S, E1-3G and E2-3G in soil are tested by a technology combining ASE (Accelerating Solvent Extraction), SPE (Solid Phase Extraction) and LC / MS / MS (Liquid Chromatography / Mass Spectrum / Mass Spectrum), and the estrogen coalitions in the deposits are extracted by using an extractant in which the ratio of acetonitrile to water (v / v) is 9:1 as an accelerating solvent. After extract is primarily purified by a NH2 column, an HLB column is used for further purification. The extract is primarily purified by the NH2 column, substances with strong nonpolarity can be removed, the influence of matrix interference on the later enrichment of the HLB column is weakened, and the purifying effect and the recovery rate are improved. The recovery rates of the four estrogen coalitions E1-3S, E2-3S, E1-3G and E2-3G with the method are all between 83% and 108%, the testing limit is lower than 0.04ng / g, and the detection requirement on the trace estrogen coalitions in the deposits or the soil samples is met.

Description

technical field [0001] The invention relates to the technical field of detection of organic pollutants in water sediment or soil, in particular to a method for extracting, purifying and detecting trace amounts of natural estrogen conjugates in sediment samples by using liquid chromatography-tandem mass spectrometry. Background technique [0002] Natural estrogens estrone (Estrone, E1), 17β-estradiol (17β-Estradiol, E2), estriol (Estriol, E3) and synthetic estrogens discharged into the water environment through human and animal feces Ethinyl estradiol (17α-Ethinyl Estradiol, EE2), is the endocrine disrupting compound (Endocrine Disrupting Compounds, EDCS) with the most potential feminizing risk, although their concentration in the water environment is only ng / L level, but It is the main substance that causes the feminization of fish. When E1, E2, and E3 are excreted from the body, the hydroxyl group at the C3- or C17-position in the estrogen molecular structure is mostly rep...

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Application Information

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IPC IPC(8): G01N30/02G01N30/14
Inventor 史江红陈庆彩吴唯刘晓薇张晖
Owner BEIJING NORMAL UNIVERSITY
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