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A detection method for phenolic endocrine disrupting substances

A technology of endocrine disruption and detection method, which is applied in the field of analysis of environmental pollutants, can solve problems such as pollution and interference with biological endocrine systems, and achieve the effects of slowing down flow speed, high selectivity and sensitivity, and strong binding ability

Active Publication Date: 2021-07-30
广州国邦检测认证有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The trade economy of the Pearl River Estuary is developed, and the proportion of industries that use EDCs as raw materials such as electronics and industry and agriculture is relatively high. The Pearl River Estuary is located in the sea-land transition zone, especially the three substances of nonylphenol, bisphenol A and triclosan. The amount of use in production is large and the use range is wide, so the direct discharge of this part of nonylphenol, bisphenol A and trichlorobiomass into the river will pose a great risk to the river and marine ecosystem of the Pearl River Estuary, causing certain pollution , and will interfere with the biological endocrine system, so it is necessary to investigate its occurrence

Method used

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  • A detection method for phenolic endocrine disrupting substances
  • A detection method for phenolic endocrine disrupting substances
  • A detection method for phenolic endocrine disrupting substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A detection method for phenolic endocrine disrupting substances, see figure 1 , including the following steps:

[0049] S001. Collection and storage of samples

[0050] When sampling, it is necessary to carry out detailed records, including the name and sample number of the sample, sampling location and latitude and longitude, sampling time, weather conditions at the time of sampling, a brief description of the sampling location, air temperature, water temperature, conductivity and pH etc.

[0051] 1) Collection of water samples

[0052] Collect four parallel 1L water samples at the same sampling point and place them in brown glass bottles respectively. When collecting water samples, take the mixed samples of the left, middle and right points 0.5cm below the horizontal plane of the same section.

[0053] Immediately add 50ml of chromatographically pure methanol and 400μL of 4mol / L sulfuric acid solution to the collected water samples, place them in a 4°C ice box, trans...

Embodiment 2

[0098] A kind of phenolic substance molecularly imprinted solid-phase extraction column, see figure 2 , including a column body 2 and a column shell 1 sleeved outside the column body 2, the column shell 1 is a hollow glass column, the column body 2 is filled in the column shell 1, and the column shell 1 is located at the bottom of the column body 2 facing the column shell 1 The center line of the cylinder shrinks, and the cylinder 2 is clamped and fixed in the cylinder shell 1 by the sieve plate 5 .

[0099] The column 2 is provided with several channels 3 for the passage of samples, and the channels 3 extend spirally from the top of the column 2 to the bottom of the column 2, and the diameter of the inlet of the channel 3 is larger than the diameter of the outlet of the channel 3.

[0100] Each channel 3 is filled with a number of flow-limiting beads 4. The composition of the flow-limiting beads 4 is polytetrafluoroethylene, and the diameter of the flow-limiting beads 4 is b...

Embodiment 3

[0106] A kind of preparation method of phenolic substance molecularly imprinted solid-phase extraction column, see figure 2 and image 3 , including the following steps:

[0107] Silica gel with a particle size of 400-600 mesh is selected as the column body 2, and several channels 3 are opened on the silica gel. The pore diameter at the top of the channel 3 is larger than that at the bottom of the channel 3.

[0108] S021. Pretreatment of silica gel surface

[0109] first through HNO 3 / H 2 Soak the silica gel in O (50ml / 50ml) to activate the hydroxyl groups on the surface of the silica gel, absorb nitric acid with deionized water, and then wash the silica gel with acetone to remove organic impurities in the silica gel. Then place it in a vacuum oven at 110°C for 12 hours to remove the physical water on the surface of the silica gel and activate the hydroxyl groups on the surface. Finally, the silica gel was removed and placed in a nitrogen-filled desiccator for later us...

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Abstract

The present invention relates to the field of analysis of environmental pollutants. Aiming at the problem of relatively large detection errors of phenolic substances, a detection method for phenolic endocrine disrupting substances is provided. The technical scheme is as follows, including the following steps: (1) Sample collection and storage; (2) sample pretreatment; (3) sample derivatization; (4) standard curve derivatization; (5) GC‑NCI‑MS analysis. Use the detection method of GC-NCI-MS to detect and analyze the samples to improve the accuracy of the analysis and detection data, and then derivatize the samples to facilitate the analysis and detection of the samples, and at the same time use the internal standard method of the standard curve to reduce the detection cost by comparison In addition, it is detected by negative chemical ionization (NCI), which has high selectivity and sensitivity to the target compound in the sample, and improves the accuracy of detection.

Description

technical field [0001] The invention relates to the field of analysis of environmental pollutants, more specifically, it relates to a detection method of phenolic endocrine disrupting substances. Background technique [0002] Environmental endocrine disrupting chemicals (Endocrine Disrupting Chemicals, EDCs) have become one of the hot environmental issues in global research because they can interfere with the endocrine system of organisms they come into contact with, and can accumulate and amplify through the food chain and eventually endanger human health. [0003] The research on EDCs by domestic scholars started relatively late, and is currently mainly focused on the investigation of the current status of use and the study of biological toxic effects, while the related research on its environmental behavior is less. The trade economy of the Pearl River Estuary is developed, and the proportion of industries that use EDCs as raw materials such as electronics and industry an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/062
Inventor 王晓燕欧阳正胡习邦黄茂生颜树涛李颖唐丽冯银坚
Owner 广州国邦检测认证有限公司
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