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A method for simultaneously detecting 7 conjugated estrogens in livestock and poultry excrements through combination of microwave extraction-solid phase extraction pretreatment and liquid chromatography-mass spectrometry technology

A technology of livestock and poultry feces and liquid mass spectrometry, which is applied in the field of detection of organic pollutant residues, to achieve the effect of improving extraction efficiency, less interference, and stable detection results

Active Publication Date: 2019-06-18
SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there is no complete and reliable detection method for the separation, enrichment and co-detection of bound estrogen in livestock and poultry feces. Therefore, there is an urgent need for a method with stable detection results, low interference, fast, efficient, sensitive and accurate detection. A method for detecting multiple bound estrogens in livestock and poultry manure, including a complete and reliable detection method for separation, enrichment and co-detection

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  • A method for simultaneously detecting 7 conjugated estrogens in livestock and poultry excrements through combination of microwave extraction-solid phase extraction pretreatment and liquid chromatography-mass spectrometry technology
  • A method for simultaneously detecting 7 conjugated estrogens in livestock and poultry excrements through combination of microwave extraction-solid phase extraction pretreatment and liquid chromatography-mass spectrometry technology
  • A method for simultaneously detecting 7 conjugated estrogens in livestock and poultry excrements through combination of microwave extraction-solid phase extraction pretreatment and liquid chromatography-mass spectrometry technology

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Effect test

Embodiment 1

[0045] Embodiment 1: standard addition recovery experiment

[0046] The influence of the microwave extraction-solid phase extraction pretreatment combined with liquid chromatography-mass spectrometry detection method of the present invention on the recovery rate of 7 kinds of bound estrogens in livestock and poultry feces was investigated by internal standard method. The recovery rate experiment of standard addition takes cow dung as an example: 100ng and 200ng of mixed standard solution (mixed standard solution is a mixed standard solution of 7 kinds of conjugated estrogens) are added to the feces respectively. Specifically follow the steps below:

[0047] Step 1. Extraction of livestock and poultry manure

[0048] The collected feces were freeze-dried, ground and passed through a sieve with a pore size of 0.25 mm. Set up two sets of stool samples for comparative test, one set is a standard sample set, the other set is a blank sample set, and each set has two parallels. Ac...

Embodiment 2-3

[0075] Example 2-3: Determination of estrogen content in actual stool samples

[0076] Determination of Concentrations of 7 Kinds of Bound Estrogens in Different Feces Samples

[0077] Collect the cow dung of three different kinds of cattle from a cattle farm in Shanghai, first adopt the method of step 1 of the present invention (microwave extraction, liquid-liquid extraction) to carry out sample pretreatment, and then use the solid phase extraction method of step 2 of the present invention to enrich After pre-purification treatment, the actual concentration of the sample is detected and analyzed by using the liquid chromatography-mass spectrometry detection method in Step 3 of the present invention, so as to investigate the applicability of the method of the present invention to different types of stool samples.

[0078] Specifically follow the steps below:

[0079] (1) Extraction of conjugated estrogen: microwave extraction

[0080] The three kinds of cow dung collected we...

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Abstract

The invention relates to a method for simultaneously detecting 7 conjugated estrogens in livestock and poultry excrements through combination of microwave extraction-solid phase extraction pretreatment and liquid chromatography-mass spectrometry technology. The method comprises the following steps: 1) carrying out pretreatment on an excrement sample, adding two internal standard substances indicating recovery rate, that is, 17beta-estradiolD3 3-beta-D-glucuronide and 17 beta-estridiol sodium sulfate-D4, then, carrying out extraction solvent microwave extraction and extraction solution filtering and collecting, and diluting the solution with water to adjust the pH value; 2)carrying out solid phase extraction enrichment and purification on target estrogens; and 3) through an internal standard method, quantitatively detecting 7 conjugated estrogens in the livestock and poultry excrements through a liquid chromatography-mass spectrometer. By optimizing the extraction method, enrichment andpurification conditions, and liquid mass testing conditions, and meanwhile, by selecting appropriate internal standard substances, the method can simultaneously detect residue information of the 7 conjugated estrogens in the livestock and poultry excrements at one time; and the method has the advantages of high recovery rate, high sensitivity, high stability, low detection limit and more realistic and reliable detection results and the like.

Description

technical field [0001] The invention belongs to the technical field of residual detection of organic pollutants, and relates to a method for detecting bound estrogen in livestock and poultry manure, in particular to a microwave extraction-solid phase extraction pretreatment combined with liquid chromatography tandem mass spectrometry technology to simultaneously detect livestock and poultry manure Method for the content of 7 kinds of conjugated estrogens. 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, and the estrogen entering the environment through livestock and poultry manure has exceeded the environmental capacity. Endogenous steroid estrogen enters the environment from the feces and urine of livestock and poultry farms, and a trace amount of endogenous steroid estrogen ca...

Claims

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Application Information

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IPC IPC(8): G01N30/08G01N30/88
Inventor 张洪昌沈根祥胡双庆郭春霞钱晓雍李贞金王真张紫琴
Owner SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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