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Method for simultaneous determination of hexabromocyclododecane isomer and tetrabromobisphenol A in fat food

A technology of hexabromocyclododecane and oily food, applied in the field of detection, can solve problems such as inapplicability, and achieve the effect of saving solvent and optimizing pretreatment technology

Inactive Publication Date: 2015-12-23
INST OF AGRI QUALITY STANDARDS & TESTING TECH RES HUBEI ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

TBBPA has relevant pretreatment methods reported for water, soil, air and other environmental matrices, such as the patent document "Selective Separation of PCNs, HBCDs and TBBPA in Complex Samples" (application number 201210103913.7, publication number CN103364238A) using silica gel as the substrate The chromatographic column packing achieves the selective separation of polychlorinated naphthalene, hexabromocyclododecane and tetrabromobisphenol A, but this method can only be used for the three types of substances in sediment, soil and biological samples For selective separation, this method is not suitable for animal food or oily samples with high fat content

Method used

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  • Method for simultaneous determination of hexabromocyclododecane isomer and tetrabromobisphenol A in fat food
  • Method for simultaneous determination of hexabromocyclododecane isomer and tetrabromobisphenol A in fat food
  • Method for simultaneous determination of hexabromocyclododecane isomer and tetrabromobisphenol A in fat food

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1 Materials and reagents:

[0035] Silica gel: silica gel (SilicaGel) 60-200 mesh. Put the silica gel into a glass chromatographic column and wash it with methanol and dichloromethane successively, and the volume of the solvent used each time is about twice the volume of the silica gel. After rinsing, place the silica gel on an aluminum foil and let it dry naturally in a fume hood, then activate it at 130°C for 4 hours, put it into a ground reagent bottle, and store it in a desiccator.

[0036] α, β, γ-hexabromocyclododecane standard solution: purity greater than 99%, all 50μg / mL, dissolved in methanol.

[0037] α, β, γ- 13 C 12 - Hexabromocyclododecane standard solution: the purity is greater than 98%, all 50μg / mL, dissolved in methanol.

[0038] Tetrabromobisphenol A standard solution: purity greater than 99%, 50 μg / mL, dissolved in methanol.

[0039] 13 C 12 -Tetrabromobisphenol A standard solution: purity greater than 99%, 50 μg / mL, dissolved in methanol.

...

Embodiment 2

[0119] The comparative test of embodiment 2 different purification methods

[0120] The following sample pretreatment method and detection method are the same as in Example 1, and the purification method is as follows:

[0121] Method 1 Acidified silica gel column purification method: put a handful of cotton at the bottom of a clean solid phase extraction glass column, pour 1cm of anhydrous sodium sulfate, 5g of silica gel, 15g of 44% acidified silica gel, 5g of silica gel, 1cm of Anhydrous Sodium Sulfate. Lightly shake the tube wall with the ear wash ball to make the packing surface level, pour n-hexane to exhaust the air bubbles, and then activate the column with 200mL n-hexane for later use.

[0122] Preparation method of 44% acidified silica gel: Weigh the activated silica gel and gradually add concentrated sulfuric acid (the mass ratio of silica gel to sulfuric acid is 44 / 56), shake overnight until there are no lumps. After completion, put it into a ground reagent bottl...

Embodiment 3Zr

[0142] Example 3ZrO 2 / mSiO 2 Composite material reusability test

[0143] 10 g of zirconia-coated mesoporous silica material (ZrO 2 / mSiO 2 ) materials were washed with 20mL acetone / ammonia water (volume ratio 95:5), 20mL acetone, and 20mL n-hexane in turn, and could be reused 5 times. The results are shown in Figure 5 .

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Abstract

The invention provides a method for simultaneous determination of hexabromocyclododecane isomer and tetrabromobisphenol A in fat food. The method is characterized by mainly including sample extraction, extract purification and determination. The extract purification uses mesoporous zirconia hybrid column as a solid phase extraction column containing an anhydrous sodium sulfate layer, a mesoporous zirconia microsphere layer, an acidified silica gel layer, a dielectric hole oxide zirconium microsphere layer and an anhydrous sulfate sodium layer from bottom to top. The recovery rate of hexabromocyclododecane isomer and tetrabromobisphenol A in plant oil, fish, meat, egg, milk and other fat food sample reaches 87.5%-114.4%. The preparation of reusable mesoporous zirconia microsphere optimizes the pretreatment technology, and saves a large amount of solvent; the detection limit, quantification limit, recovery rate and precision can meet the requirements for analysis of real samples; and reliability of the method and result accuracy are verified through the standard substance in international comparison.

Description

technical field [0001] The invention relates to a detection method, in particular to a method for simultaneously measuring the content of hexabromocyclododecane isomers and tetrabromobisphenol A in oily foods. Background technique [0002] Hexabromocyclododecanes (HBCDs): 1,2,5,6,9,10-Hexabro, CAS number: 3194-55-6, molecular weight: 641.70, molecular formula: C 12 h 18 Br 6 . [0003] Tetrabromobisphenol A (TetrabromobisphenolA, TBBPA): 3,3,5,5-Tetrabromobi, CAS number: 79-94-7, molecular weight: 543.87, molecular formula: C 15 h 12 Br 4 o 2 . [0004] Hexabromocyclododecane and tetrabromobisphenol A are two brominated flame retardants with the largest consumption in the world, and are widely used in polymer production, flame retardant printed circuit boards, building insulation boards, upholstered furniture, indoor Decorative textiles and other fields. In 2010, the global production of HBCDs was 23,000 tons, and in 2004, the global production of TBBPA was 170,000 ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 龚艳彭西甜闻胜彭立军张兴中
Owner INST OF AGRI QUALITY STANDARDS & TESTING TECH RES HUBEI ACADEMY OF AGRI SCI
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