Process for jointly detecting estrogens and their associations in livestock and poultry excrements

A technology of livestock and poultry manure and a detection method, which is applied in the field of liquid chromatography-tandem mass spectrometry combined detection, can solve the problems of the presence of trace amounts of estrogen and its conjugates, large matrix interference, and difficult pretreatment technology, and reaches the detection limit. Low, high sensitivity, simple and easy to operate

Inactive Publication Date: 2012-10-17
BEIJING NORMAL UNIVERSITY
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Problems solved by technology

[0005] The purpose of the present invention is to develop a high recovery rate, high sensitivity, accurate and fast analysis method for the problems of trace amounts of estrogen and conjugates in livestock and poultry feces sa

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  • Process for jointly detecting estrogens and their associations in livestock and poultry excrements
  • Process for jointly detecting estrogens and their associations in livestock and poultry excrements
  • Process for jointly detecting estrogens and their associations in livestock and poultry excrements

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Embodiment Construction

[0043] Below in conjunction with example and accompanying drawing, technical scheme of the present invention is described further

[0044] (1) Solid sample extraction

[0045] Freeze-dry the collected livestock and poultry feces samples, accurately weigh 0.5g of the sample, use 66mL of acetone / methanol=1:1 (v / v) as the extraction solvent, and use the fast solvent extraction method to extract the estrogen and its conjugates in the sample ; Then concentrated by rotary evaporation to about 1mL, blown dry with nitrogen, and kept the residue for purification. The temperature selected for the fast solvent extraction method of the present invention is 80° C., the pressure is 1500 psi, and static extraction is performed twice, each for 8 minutes.

[0046] (2) Sample pre-purification

[0047] a. Liquid-liquid extraction and purification: re-dissolve the residue with 5 mL of acetonitrile, then add 10 mL of n-hexane and vortex mix for 5 minutes, liquid-liquid extraction to remove greas...

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Abstract

The invention relates to a technology for detecting endocrine disrupters in the environment, and especially relates to a technology for quantitatively analyzing estrone (E1), 17beta-estradiol (E2), estriol (E3), 17alpha-ethinyl estradiol (EE2), estrone-3-glucuronide (E1-3G), 17beta-estradiol-3-glucuronide (E2-3G), estrone-3-sulfate (E1-3S) and 17beta-estradiol-3-sulfate (E2-3S) in a complex matrix livestock and poultry excrement sample through adopting a liquid chromatography-tandem mass spectrometry technique. The technology comprises the following steps: extracting estrogens in the collected livestock and poultry excrement sample through adopting a rapid solvent extraction method, pre-purifying the resulting extract through liquid-liquid extraction and alkaline solution extraction, enriching targets with an HLB column, purifying estrogen monomers and estrogen associations through using a Florisil column and an NH2 column respectively, and finally detecting through adopting the liquid chromatography-tandem mass spectrometry technique. The process has the advantages of environmental pollution, easy operation, and high recovery rate, and allows the estrogens and their associations having trace amounts in the complex matrix livestock and poultry excrements to be rapidly analyzed.

Description

technical field [0001] The invention relates to the technical field of liquid chromatography-tandem mass spectrometry detection, in particular to the extraction, purification and instrument detection methods of estrogen and its conjugates in complex livestock and poultry feces samples. Background technique [0002] In recent years, natural and synthetic estrogens estrone (Estrone, E1), 17β-estradiol (17β-Estradiol, E2), estriol (Estriol, E3) and 17α-ethinyl estradiol (17α-Ethinyl Estradiol , EE2) as a typical environmental endocrine disruptor has aroused widespread concern in the academic community. Relevant investigations and studies have shown that the ng / L concentration level in the water environment can pose a feminization risk to aquatic organisms such as fish. The urine and feces discharged by humans and mammals are the most fundamental sources of estrogen in the environment, and their discharge is inevitable. Estrogen is metabolized by the liver, and is mainly excre...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 史江红吴唯张晖刘晓薇陈庆彩薄婷贾彦舶
Owner BEIJING NORMAL UNIVERSITY
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