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A method for measuring hexabromocyclododecane isomers in plants

A technology of hexabromocyclododecane and isomers, which is applied in the field of determination of hexabromocyclododecane isomers in plants, can solve the problems of limited analysis and determination methods, and achieve low detection limit, high sensitivity and high recovery rate. high effect

Active Publication Date: 2020-05-19
SOUTH CHINA SEA INST OF OCEANOLOGY - CHINESE ACAD OF SCI
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Problems solved by technology

[0003] At present, the research reports on the analysis and determination methods of HBCD mainly focus on soil, sediment and animal bodies, and the analysis and determination methods of HBCD stereo and enantiomers in plants are still very limited.

Method used

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  • A method for measuring hexabromocyclododecane isomers in plants
  • A method for measuring hexabromocyclododecane isomers in plants
  • A method for measuring hexabromocyclododecane isomers in plants

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Embodiment 1

[0040] 1. Determination and analysis method

[0041] (1) Preparation before experiment

[0042] a. Paper tube: Cut the filter paper to a suitable size, roll it up and tie it tightly with a thin thread, extract it with dichloromethane for 24 hours, then replace it with new dichloromethane and continue the extraction for 24 hours.

[0043] b. Silica gel: Put 80-100 mesh silica gel into the paper tube, extract with dichloromethane Soxhlet for 24 hours, replace with new dichloromethane and continue to extract for 24 hours; after air drying, put it in a crucible, and put it in an oven at 180°C for continuous extraction Activate for 12 hours, remove carbon black and other impurities after cooling to room temperature, put into a flat-bottomed flask and weigh; add 3% silica gel weight deionized water drop by drop to deactivate, shake until there are no hardened particles, and equilibrate overnight. Add enough n-hexane to the neutral silica gel to ensure that the silica gel is complet...

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Abstract

The invention discloses a method for determining hexabromocyclododecane isomers in plants. The method comprises the following steps: adding a recovery indicator for Soxhlet extraction, performing liquid-liquid extraction with concentrated sulfuric acid and normal hexane, purifying the extracting solution by adopting a multilayer silica gel composite column, adding an internal standard substance, and detecting and analyzing HBCD (hexabromocyclododecane) stereisomers and enantiomers by using a high performance liquid chromatograph-triple quadrupole mass spectrometry system. The method disclosedby the invention is capable of accurately performing purification treatment and qualitative and quantitative analytical determination on the HBCD stereisomers and enantiomers in plant samples, and isapplicable to formulation of standardization.

Description

technical field [0001] The invention belongs to the technical field of organic pollutant analysis and detection, and in particular relates to a method for measuring hexabromocyclododecane isomers in plants. Background technique [0002] Hexabromocyclododecane (HBCD, C 12 h 18 Br 6 ) As an additive brominated flame retardant, it is widely used in building thermal insulation materials, textiles, plastics, and electronic and electrical products because of its small dosage, good flame retardant effect, and little impact on the physical properties of materials. There are 16 isomers in HBCD theory, including 6 pairs of enantiomers and 4 axisymmetric isomers. Currently, 8 isomers have been separated: 3 pairs of enantiomers (±)-α -, β- and γ-HBCD and δ- and ε-HBCD. HBCD in industrial products is mainly composed of three isomers of α-, β- and γ-HBCD, and their proportions are 10-13%, 1-12% and 75-89%, respectively, and the three isomers are all racemate (enantiomeric fraction, E...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 孙毓鑫李华薇胡咏霞汪伟薇徐向荣
Owner SOUTH CHINA SEA INST OF OCEANOLOGY - CHINESE ACAD OF SCI
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