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Method for detecting 10 halogenated carbazole compounds in marine sediments

A technology for marine sediments and substituted carbazoles, which is applied in the field of marine sediment detection, can solve the problems of unknown properties of halogenated carbazoles and limited halogenated carbazoles, and achieve the promotion of quality and safety, high sensitivity, and increased The effect of export volume

Active Publication Date: 2022-07-29
ZHOUSHAN INST FOR FOOD & DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] With the continuous research and exploration of halogenated carbazoles, more than 20 kinds of halogenated carbazoles have been detected in the environment so far, but as a new type of pollutants, many properties of halogenated carbazoles are still unknown
So far, the knowledge about the toxicological properties and environmental behavior of halogenated carbazoles is still very limited, and the research on its pollution is mainly concentrated in water and soil, and there are relatively few studies in marine sediments and marine organisms.

Method used

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  • Method for detecting 10 halogenated carbazole compounds in marine sediments
  • Method for detecting 10 halogenated carbazole compounds in marine sediments
  • Method for detecting 10 halogenated carbazole compounds in marine sediments

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Embodiment 1

[0058] 1. A method for detecting 10 halogenated carbazole compounds in marine sediments, comprising:

[0059] 1.1 Configuration standard product:

[0060] Weigh the above 10 standard halogenated carbazole compounds of the same mass and mix them, and prepare a mixed solution with a mass concentration of 1000 mg / L using acetone as a solvent. Prepare 10mg / L standard stock solution and store at -20℃; Dilute the standard stock solution with acetone to the concentration of 0.1ng / mL, 0.2ng / mL, 0.5ng / mL, 1ng / mL, 2ng / mL respectively , 5ng / mL, 10ng / mL, 20ng / mL, 50ng / mL, 100ng / mL to obtain a standard series of working solutions, which were stored in a -20°C refrigerator away from light until testing.

[0061] 1.2 Sample collection and processing:

[0062] Sediment samples were collected at the sampling point. The collected sediment samples were first removed of impurities, freeze-dried and placed in a stainless steel box, ground at 30°C, passed through an 80-mesh sieve, freeze-dried, a...

Embodiment 2

[0088] 1.3.1 Preparation of silica gel microspheres: Mix 60 mL of water, 20 mL of ethanol, and 14 mL of 0.67 mol / L ammonia water evenly, add 15 mL of ethyl orthosilicate dropwise with stirring, and stir for 20 h in a water bath at 25 °C. Under the condition of 48 ℃ water bath, vacuum and rotary steam for 2 hours to obtain silica sol; dilute the silica sol to 130 mL, add 0.3 g of diethylene glycol ether, 1.8 g of formaldehyde, and 4.5 g of urea, stir to completely dissolve, and add hydrochloric acid solution to adjust the value To 1.6, let stand, add enough deionized water to stop the reaction after the solution turns completely white, stand for 12 hours, filter the white precipitate at the bottom, wash with water and ethanol in turn, dry in a vacuum drying oven at 90°C for 24h, 110°C Dry for 24h, then put it into a muffle furnace for calcination, keep at 150°C for 4h, 250°C for 6h, 350°C for 8h, 450°C for 10h, and 550°C for 12h to obtain white silica gel microspheres. The rest...

Embodiment 3

[0090] 1.3.1 Preparation of silica gel microspheres: Mix 60 mL of water, 20 mL of ethanol, and 14 mL of 0.67 mol / L ammonia water evenly, add 15 mL of ethyl orthosilicate dropwise with stirring, and stir for 20 h in a water bath at 25 °C. Under the condition of 48 ℃ water bath, vacuum and rotary steam for 2 hours to obtain silica sol; dilute the silica sol to 130 mL, add 1.5 g of diethylene glycol ether, 1.8 g of formaldehyde, and 4.5 g of urea, stir to dissolve it completely, and add hydrochloric acid solution to adjust the value To 1.6, let stand, add enough deionized water to stop the reaction after the solution turns completely white, stand for 12 hours, filter the white precipitate at the bottom, wash with water and ethanol in turn, dry in a vacuum drying oven at 90°C for 24h, 110°C Dry for 24h, then put it into a muffle furnace for calcination, keep at 150°C for 4h, 250°C for 6h, 350°C for 8h, 450°C for 10h, and 550°C for 12h to obtain white silica gel microspheres. The r...

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Abstract

The invention provides a method for detecting 10 halogenated carbazole compounds in marine sediments, which belongs to the technical field of marine sediment detection, and comprises the following steps: extracting and purifying a to-be-detected sample by using self-made C18 bonded silica gel as an auxiliary agent, separating a standard substance or the to-be-detected sample by using a chromatographic column, retaining the standard substance or the to-be-detected sample in a mass spectrum, collecting accurate mass numbers, and determining the content of the halogenated carbazole compounds in the marine sediments. And optimizing the mass spectrum voltage, scanning and collecting parameters, and carrying out accurate qualitation and quantification on the 10 halogenated carbazole compounds. According to the method, the extraction effect of the halogenated carbazole compounds is improved by improving a C18 bonded silica gel preparation method, and then the halogenated carbazole compounds in the marine sediments are detected by utilizing qualitative and quantitative functions of gas chromatography-triple quadrupole tandem mass spectrometry. The method has the advantages of simplicity, convenience and rapidness in operation, capability of effectively reducing interference of matrix components, high sensitivity, high resolution and the like.

Description

technical field [0001] The invention belongs to the technical field of marine sediment detection, in particular to a method for detecting 10 halogenated carbazole compounds in marine sediments. Background technique [0002] Carbazole (9H-Carbazole, CZ, molecular formula C 12 H 9 N) and its derivatives are a class of nitrogen-containing heterocyclic aromatic hydrocarbon compounds, which are widely used in many fields such as optoelectronic materials, dyes, medicine and supramolecular recognition. Polyhalogenated 9H-carbazoles (PHCZs) refer to a class of compounds in which the hydrogen atoms on the carbazole ring are replaced by halogen atoms (Cl, Br or I). PHCZs are a new class of organic pollutants similar in structure to polychlorinated dibenzofurans. In recent years, it has been defined as a potentially persistent, bioaccumulative toxic substance (PBT) by the European Commission. Toxicological studies have shown that exposure to carbazoles and halocarbazoles has advers...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/08G01N30/14G01N30/72G01N30/86
CPCG01N30/06G01N30/08G01N30/14G01N30/7206G01N30/8679G01N2030/047G01N2030/062G01N2030/146
Inventor 唐雷鸣蒋玲波陈翔高卓瑶王萍亚赵巧灵戴意飞刘婷
Owner ZHOUSHAN INST FOR FOOD & DRUG CONTROL
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