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Method for extracting and determining hexabromocyclododecanes in plant-soil system

A technology of hexabromocyclododecane and plants, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high extraction temperature, decomposition of extracts, expensive equipment, etc., achieve good extraction effect, reduce loss process, reduce The effect of the action steps

Inactive Publication Date: 2017-08-08
SOUTH CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of Soxhlet extraction is high recovery rate; ultrasonic extraction is cheap and fast, but the operation is relatively cumbersome and the recovery rate is low; microwave extraction takes a short time, high recovery rate, and less solvent consumption, but the extraction temperature is higher, which may cause The extract is decomposed, and the equipment is more expensive

Method used

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  • Method for extracting and determining hexabromocyclododecanes in plant-soil system
  • Method for extracting and determining hexabromocyclododecanes in plant-soil system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A method for extracting and measuring hexabromocyclododecane in a plant-soil system, comprising the steps of:

[0038] S1. Pick and wash the plants to be tested, separate the roots, stems and leaves, dry them in an oven, and crush them with a plant breaker to become a plant sample to be tested; the soil is naturally air-dried, passed through a 2mm sieve, and weeds and other impurities are removed. Become the sample to be tested of soil;

[0039] S2. Weigh 5g of the plant / soil sample to be tested and put it into a pure filter paper tube, add 4 drops of n-hexane into the filter paper tube, and add a small ball of absorbent cotton above the sample.

[0040] S3. Add 150ml of n-hexane-acetone (1:3, v / v) into the round bottom flask for Soxhlet extraction for 12h, the solvent reflux rate is controlled at reflux 6 times per hour, and then the extract solution is rotary evaporated to near dryness; add 15ml Dissolve concentrated sulfuric acid and 5ml of n-hexane, transfer the so...

Embodiment 2

[0042] A method for extracting and measuring hexabromocyclododecane in a plant-soil system, comprising the steps of:

[0043] S1. Pick and wash the plants to be tested, separate the roots, stems and leaves, dry them in an oven, and crush them with a plant breaker to become a plant sample to be tested; the soil is naturally air-dried, passed through a 2mm sieve, and weeds and other impurities are removed. Become the sample to be tested of soil;

[0044] S2. Weigh 5g of the plant / soil sample to be tested and put it into a pure filter paper tube, add 3 drops of n-hexane into the filter paper tube, and add a small ball of absorbent cotton above the sample.

[0045] S3. Add 150ml of n-hexane-acetone (1:2, v / v) to the round bottom flask for Soxhlet extraction for 14h, the solvent reflux rate is controlled at reflux 5 times per hour, and then the extract is rotary evaporated to near dryness; add 25ml Dissolve concentrated sulfuric acid and 5ml of n-hexane, transfer the solution to a c...

Embodiment 3

[0047] A method for extracting and measuring hexabromocyclododecane in a plant-soil system, comprising the steps of:

[0048] S1. Pick and wash the plants to be tested, separate the roots, stems and leaves, dry them in an oven, and crush them with a plant breaker to become a plant sample to be tested; the soil is naturally air-dried, passed through a 2mm sieve, and weeds and other impurities are removed. Become the sample to be tested of soil;

[0049] S2. Weigh 5g of the plant / soil sample to be tested and put it into a pure filter paper tube, add 4 drops of n-hexane into the filter paper tube, and add a small ball of absorbent cotton above the sample.

[0050] S3. Add 150ml of n-hexane-acetone (1:4, v / v) to the round bottom flask for Soxhlet extraction for 16h, the solvent reflux rate is controlled at reflux 5 times per hour, and then the extract is rotatably evaporated to near dryness; add 20ml Dissolve concentrated sulfuric acid and 5ml of n-hexane, transfer the solution t...

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Abstract

The invention discloses a method for extracting and determining hexabromocyclododecanes in a plant-soil system. The method comprises the following steps: S1, pretreating a to-be-detected plant / soil sample; S2, adding the to-be-detected plant / soil sample into a filter paper barrel, adding 3 to 4 drops of normal hexane, and adding a small piece of degreasing cotton above the sample; S3, performing Soxhlet extraction for 12 to 16h by taking normal hexane-acetone of which the volume ratio is 1:1 as a solvent, performing reflux for 5 to 7 times every hour, evaporating an extracting solution until the extracting solution is nearly dried, adding concentrated sulfuric acid and normal hexane of which the volume ratio is (3 to 5):1 for dissolving, extracting liquid supernatant after centrifugation, performing solid-phase extraction on the liquid supernatant through a solid-phase extraction column, and collecting eluant; then evaporating and concentrating the eluant until the eluant is nearly dried, cleaning by using methyl alcohol, nitrogen-blowing the eluant until the eluant is dried, fixing volume by using the methyl alcohol, performing full and uniform mixing, and determining by using high performance liquid chromatography-mass spectrometry. The method has the advantages of high determination speed, accurate analysis result, low pretreatment cost and applicability to migration and evaluation of a hexabromocyclododecane isomer in the plant-soil system.

Description

technical field [0001] The invention belongs to the technical field of organic pollutant detection, and in particular relates to a method for extracting and measuring hexabromocyclododecane in a plant-soil system. Background technique [0002] Since the 1960s, hexabromocyclododecanes (HBCDs) have been added to extruded and expanded polystyrene materials (addition <3%) and are widely used in the construction industry, textile industry and electronics. industry. In 2001, the global production of HBCDs reached 16,700 tons, second only to tetrabromobisphenol-A (>130,000 tons) and decabromobiphenyl acid (56,100 tons), becoming the third largest brominated flame retardants (BFRs). In 2009, after Pentabromodiphenyl Ether and Octabromodiphenyl Ether were banned, HBCDs became their substitute, and the output rose rapidly. [0003] However, studies have shown that HBCDs also exhibit the characteristics of persistence, long-distance migration, high enrichment and toxicity in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 吕辉雄马晓净周耀红陈少华李军辉黄雪晶郑丽
Owner SOUTH CHINA AGRI UNIV
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