Method using microwave extraction-solid phase extraction pretreatment combined high performance liquid chromatography-mass spectrometry technology to simultaneously detect three-category 6 estrogens in livestock and poultry manure

Abstract

The invention provides a method using the microwave extraction-solid phase extraction pretreatment combined high performance liquid chromatography-mass spectrometry technology to simultaneously detectthree-category 6 estrogens in livestock and poultry manure. The method includes the steps of firstly, pretreating a manure sample, and adding an internal standard substance before the adding of an extraction solvent to indicate the recycling rate; secondly, using a microwave extraction instrument to extract the target estrogens in the manure sample; thirdly, using a solid phase extraction columnto enrich and purify the target estrogens; fourthly, using an internal standard method and a high performance liquid chromatography-mass spectrometry instrument to detect the content of the three-category 6 estrogens in the manure sample. The method has the advantages that the single-factor experiment is used, the extraction method and the extraction solvent are optimized, and the residue conditions of the three-category 6 estrogens in chicken manure, cattle manure and pig manure can be simultaneously in one step; the internal standard substance for indicating the recycling rate is added before the microwave extraction, target substance loss during pretreatment can be well indicated, and the final result is real and reliable.

Description

technical field [0001] The invention belongs to the technical field of residual detection of organic pollutants in livestock and poultry manure, relates to a method for detecting estrogen in livestock and poultry manure, in particular to a microwave extraction-solid phase extraction pretreatment combined with liquid chromatography tandem mass spectrometry ( HPLC-MS / MS, referred to as liquid mass spectrometry), is a method that can efficiently process and simultaneously detect three types of 6 estrogens in livestock and poultry manure. technical background [0002] With the rapid development of the livestock and poultry breeding industry in the direction of modernization, scale and intensification, the pollution of livestock and poultry breeding is becoming more and more serious. 90% of the total natural estrogen in the environment comes from large-scale intensive livestock and poultry farming, including the use of hormone drugs, livestock and poultry feed additives, and the ...

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the problems of instability, interference, limited amount of estrogen detection and recovery rate in the existing methods, and to provide a method with accurate and stable detection results, low interference, fast and efficient, and simultaneous determination of estrogen. Three types of estrogens (natural estrogens, synthetic estrogens, and endocrine disruptors with estrogenic effects) in livestock and poultry manure (chicken manure, cow manure, pig manure) and 6 kinds of estrogens with different structures (estrone, estradiol , estriol, ethinyl estradiol, diethylstilbestrol, bisphenol A), that is, a simultaneous detection of livestock and poultry feces by microwave extraction, solid phase extraction pretreatment combined with high performance liquid chromatography tandem mass spectrometry (HPLC-MS / MS) Method of 6 kinds of estrogen in three categories

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