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Method for simultaneously detecting nine types of oestrogen substances in water by solid phase extraction-liquid chromatography-tandem mass spectrometry

A technology of liquid chromatography and tandem mass spectrometry, which is applied in the field of simultaneous detection of 9 estrogen substances in water by solid phase extraction-liquid chromatography tandem mass spectrometry, can solve the problem of limited quantity and range of estrogen detection, inaccurate detection results, Problems such as large consumption of organic reagents can achieve the effects of saving manpower and material costs, less time consumption and high recovery rate

Inactive Publication Date: 2018-01-05
SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the existing solid-phase extraction combined with liquid chromatography-mass spectrometry is used for the detection of estrogens in the water environment, most of them are due to poor pretreatment, or the pretreatment conditions of solid phase extraction, liquid chromatography conditions and / or mass spectrometry The conditions are not well selected, and there are more or less problems such as inaccurate test results, instability, excessive interference, large consumption of organic reagents, limited quantity and range of estrogen detection, etc.

Method used

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  • Method for simultaneously detecting nine types of oestrogen substances in water by solid phase extraction-liquid chromatography-tandem mass spectrometry
  • Method for simultaneously detecting nine types of oestrogen substances in water by solid phase extraction-liquid chromatography-tandem mass spectrometry
  • Method for simultaneously detecting nine types of oestrogen substances in water by solid phase extraction-liquid chromatography-tandem mass spectrometry

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Embodiment 1

[0035] Example 1: A method of the present invention for the simultaneous determination of 9 estrogen substances in water by solid phase extraction-liquid chromatography tandem mass spectrometry is specifically implemented as follows:

[0036] Step one, water sample pretreatment

[0037] The volume required for different types of water samples is different. Tap water and river water are respectively 1L; livestock and poultry farm sewage is 0.1L, centrifuged to remove large suspended solids and diluted with Mliil-Q ultrapure water 10 times to 1L. Use Whatman GF / F series of 0.45um glass fiber membrane to filter, collect the filtered water sample, add 100ng of 17β-estradiol-d3 (17β-E2-d3), diethylstilbestrol-D8 (DES-D8) ), 4n-nonylphenol-D8 (4n-NP-D8), the three internal standards indicating the recovery rate, after mixing, adjust the pH of the water sample to 3-4 with 4mol / L dilute hydrochloric acid.

[0038] Step two, solid phase extraction pretreatment: enrichment purification proces...

Embodiment 2-3

[0076] Example 2-3: Measurement of actual environmental samples

[0077] Determination of the concentration of 9 estrogen substances in two different actual water bodies

[0078] Collect surface water samples from rivers around a livestock farm in Shanghai and sewage effluent from a dairy farm. First, use the method of step 1 in Example 1 for pretreatment, and then use the method of step 2 of Example 1 for solid-phase extraction, enrichment and purification. After that, the detection method established in step 3 of embodiment 1 was used to detect and analyze the actual concentration of the sample to investigate the applicability of the detection method established in step 3 of embodiment 1 of the present invention.

[0079] The contents of 9 estrogen substances in the two water samples obtained from the actual test are shown in Table 4 below. The experimental results show that the method of the present invention can be applied to the determination of estrogen content in conventional...

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Abstract

The invention discloses a method for simultaneously detecting nine types of oestrogen substances in water by solid phase extraction-liquid chromatography-tandem mass spectrometry. The method comprises(1) carrying out water sample pretreatment, (2) enriching and purifying a target oestrogen with a solid phase extraction small column and (3) quantificationally detecting nine types of oestrogen substances in water through an internal standard method through a high efficiency liquid chromatography-tandem mass spectrometer. The method utilizes a single factor test, optimizes the type of a solid phase extraction small column, pH in solid phase extraction, the type and use amount of an eluting agent and the type and use amount of an eluent, optimizes a liquid chromatographic column temperature,a flowing rate, a sample loading amount, a flowing amount, the fluid type and a gradient ratio, has short peak production time and produces an ion chromatogram having a good separation degree. The method utilizes the internal standard substance indicating a recovery rate before solid phase extraction, well shows the loss of the target substances in the pretreatment and produces a real and reliablefinal result.

Description

Technical field [0001] The invention belongs to the technical field of safety detection of trace organic pollutant residues in water environments, relates to pretreatment methods and instrument detection and analysis techniques for 9 conventional estrogen substances in three water environments, and specifically relates to a solid phase extraction-liquid chromatography Tandem mass spectrometry is a method for the simultaneous detection of 9 estrogen substances in water. technical background [0002] In recent years, environmental endocrine disruptors (EDCs) have attracted widespread attention. Studies have shown that EDCs can induce feminization of male fish, affect the growth and reproduction of aquatic organisms, and increase the incidence of human breast cancer. Natural and synthetic estrogens are the most important EDCs. They have the strongest endocrine disrupting properties, and the nanogram level is sufficient to cause adverse effects on aquatic organisms. Natural estrogen...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08
Inventor 张洪昌沈根祥胡双庆钱晓雍王振旗朱英袁哲军张玉
Owner SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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