Method for analyzing and determining organics persistently containing chlorine in aquatic product

A method of determination and technology of aquatic products, applied in the field of chemical analysis, can solve the problems of ineffective removal of impurity interference, complicated background of chlorine-containing compounds, and unguaranteed reliability of the method, achieving a high degree of column commercialization and a high degree of automation , Labor saving effect

Inactive Publication Date: 2010-08-25
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The difficulties in carrying out the analysis and determination include: 1. The content of chlorinated organic compounds in fish and aquatic products is trace, and the detection limit of the instrument usually cannot reach; 2. Whether the recovery rate of chlorinated compounds in the whole process can be Ideal, that is, the reliability of the method cannot be guaranteed; 3. The background of chlorine-containing compounds is complex (that is, there are many compounds in organisms such as fish that interfere), and impurities and interferences cannot be effectively removed)

Method used

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  • Method for analyzing and determining organics persistently containing chlorine in aquatic product
  • Method for analyzing and determining organics persistently containing chlorine in aquatic product
  • Method for analyzing and determining organics persistently containing chlorine in aquatic product

Examples

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Effect test

Embodiment 1

[0040] The present invention is used to analyze the wild whitebait in South Taihu Lake, Huzhou City, Zhejiang Province, and determine the types and contents of chlorine-containing organic matter therein.

[0041] The whitebait samples stored at -20°C were taken out from the refrigerator and thawed at room temperature. The whole fish was freeze-dried for 48 hours, and the dried samples were ground with an agate mortar.

[0042] Two samples of 3.0 g were accurately weighed by an electronic balance, and continuously Soxhlet-extracted with a mixture of 100 mL of n-hexane and acetone (volume ratio 1:1). The heating plate temperature of the Soxhlet extractor is 63°C, and the automatic extraction time is 960min. One part of the extract was measured by gravimetric method for the fat content of whitebait, and the other part was filtered through absorbent cotton with anhydrous sodium sulfate to remove a small amount of water and solid impurities.

[0043] The extract is then purified ...

Embodiment 2

[0048] The present invention is used to analyze the wild whitefish of South Taihu Lake in Huzhou City, Zhejiang Province, and determine the types and contents of chlorine-containing organic matter therein.

[0049] The white fish samples stored at -20°C were taken out from the refrigerator and thawed at room temperature. The back muscle of white fish was taken and freeze-dried for 48 hours. After drying the samples were ground with an agate mortar.

[0050] Two samples of 3.0 g were accurately weighed by an electronic balance, and continuously Soxhlet-extracted with a mixture of 100 mL of n-hexane and acetone (volume ratio 1:1). The heating plate temperature of the Soxhlet extractor is 63°C, and the automatic extraction time is 960min. One part of the extract was measured by gravimetric method for the fat content of white fish, and the other part was filtered through absorbent cotton with anhydrous sodium sulfate to remove a small amount of water and solid impurities.

[00...

Embodiment 3

[0056] The invention is used to analyze a certain fish muscle tissue provided by the United Nations Environment Program (UNEP), and to determine the type and content of chlorine-containing organic substances therein.

[0057] An electronic balance accurately weighed 2.5 g of the dried and ground sample, and extracted it with 100 mL of a mixture of n-hexane and acetone (1:1 by volume) for continuous Soxhlet extraction. The heating plate temperature of the Soxhlet extractor is 63°C, and the automatic extraction time is 960min. The extract is filtered with absorbent cotton with anhydrous sodium sulfate to remove a small amount of water and solid impurities.

[0058] The extract is then purified by a gel chromatograph to remove large molecular weight substances. The solvent is concentrated to 8mL during the single concentration procedure, and the solvent is replaced with n-hexane and concentrated to 4mL during the double machine procedure; then the purified solution Concentrate t...

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Abstract

The invention discloses a method for analyzing and determining organics persistently containing chlorine in an aquatic product, and the method comprises the following steps of: A) drying and grinding muscle tissues in the aquatic product; B) Soxhlet extraction; C) gel permeation chromatographic purification; D) degreasing by concentrated sulfuric acid; E) chromatography by a Florisil chromatographic column; and F) determining the organics persistently containing chlorine by a gas chromatography method. In the method, sample extraction and purification operation are simple, the solvent consumption is little, the analysis speed is fast, both properties and quantities of 40 types of organics persistently containing chlorine can be determined accurately, the detection limits are low, the sensitivity is high, and the detection limits are all lower than 4ng/g-lw.

Description

technical field [0001] The invention belongs to the field of chemical analysis, and relates to an analysis and determination method for organic pollutants, in particular to an analysis and determination method for persistent chlorine-containing organic substances in aquatic products. Background technique [0002] Persistent chlorinated organic compounds mainly include organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs), among which hexahexysix (HCHs), DDTs (DDTs), chlordane, aldrin, dieldrin, endrin , hexachlorobenzene (HCB), polychlorinated biphenyls (PCBs), etc. have been included in the Stockholm Convention on Persistent Organic Pollutants (POPs) and the blacklist of priority pollutants in various countries around the world. Organochlorine pesticides are mainly used to prevent and control harmful organisms in agricultural production, and PCBs are widely used in the fields of electric power industry, plastic processing industry, chemical industry and prin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N1/28G01N1/34
Inventor 仇雁翎李力朱志良程炳宏郑阳华赵建夫
Owner TONGJI UNIV
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