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Detection method for content of brominated flame retardants (BFRs) in food

A brominated flame retardant and detection method technology, applied in the detection field of brominated flame retardant content in food, can solve the problem of increasing the loss of target objects and the intensity of experiments, increasing the risk of decomposition of high-brominated substances, and large baseline interference and other problems, to achieve the effect of preventing degradation, high sensitivity, and overcoming cumbersome steps

Active Publication Date: 2018-12-21
SUZHOU UNIV OF SCI & TECH
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  • Summary
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  • Application Information

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Problems solved by technology

The invention has high sample extraction efficiency, but the method takes a long time to extract, which increases the risk of decomposition of highly brominated substances such as DBDPE and BDE209
In October 2011, Marine Environmental Science published the "Analysis Method of Polybrominated Diphenyl Ethers and Polybrominated Biphenyls in Marine Biological Samples", using ultrasonic extraction, and the extract was purified by acid silica gel and neutral silica gel chromatography column combined with gas chromatography-negative ion chemical source (NCI) / Mass spectrometry analysis of 5 polybrominated biphenyl (ether) residues including BDE-47, BDE-99, BDE-100, BDE-153 and BDE154 in various fish and shellfish, but not for high brominated BDE209 and DBDPE
Microwave-assisted extraction has been widely used in the extraction of polybrominated diphenyl ethers in solid matrices such as soil or sediment, but there are few research reports on the microwave extraction of PBDEs residues in poultry eggs and other foods, so it is of great significance to establish a method for the determination of this aspect
[0004] In addition, poultry eggs contain high protein and fat, which greatly interferes with the baseline, and they need to be purified before they can be analyzed by instruments. The traditional purification methods include concentrated sulfuric acid for fat removal, gel permeation chromatography column, and solid phase extraction column purification. This method has a large amount of fat removal, but requires more steps of extraction, filtration and solvent conversion, which increases the loss of the target and the intensity of the experiment

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  • Detection method for content of brominated flame retardants (BFRs) in food
  • Detection method for content of brominated flame retardants (BFRs) in food
  • Detection method for content of brominated flame retardants (BFRs) in food

Examples

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Effect test

Embodiment 1

[0057] This embodiment focuses on GC-NCI-MS analysis of 13 kinds of brominated flame retardants to ensure the accuracy of qualitative and quantitative.

[0058] Step 1: Use BDE-CSM PBDE8 mixed standard, BDE-203, BDE-206, BDE-207, BDE-208 and DBDPE single standard purchased from Bailingwei Technology Co., Ltd., with a concentration of 1000mg / L. Alkanes are formulated into PBDEs (low brominated BDEs: BDE-28, BDE-47, BDE-99, BDE-100, BDE-153, BDE-154, BDE-183) with a standard working curve concentration of 0.5, 1.0, 5.0, 10.0 and 50.0μg / L, high bromine-BDE (BDE-203, BDE-206, BDE-207, BDE-208) standard working curve concentration is 1.0, 5.0, 10.0, 50.0 and 100.0μg / L, BDE209 and DBDPE standard The working curve concentration is the mixed standard working solution of 5.0, 10.0, 50.0, 100.0 and 500.0 μg / L.

[0059] Step 2: Set gas chromatography-mass spectrometry conditions: select DB-5HT capillary column (15m×0.25mm i.d., 0.10μm, Agilent); splitless injection, injection volume 1.0...

Embodiment 2

[0065] This example focuses on the microwave-assisted extraction of 13 brominated flame retardants in poultry eggs, and optimizes the conditions of the microwave-assisted extraction.

[0066] Step 1: Wash the surface of the egg, dry it in the air, remove the shell, mix the egg yolk and egg white, freeze it at -20°C to become solid, then place it in a freeze dryer, and vacuum freeze-dry it at -55°C for 24 hours. Grind into powder, mix 1.0g of egg samples with 5.0g of anhydrous sodium sulfate, completely transfer to a 100ml polytetrafluoroethylene extraction tube, add 13 kinds of standard samples (50ng / g) of the analyte, shake and mix, Equilibrate for 3h.

[0067] Step 2: Add 30ml of n-hexane / acetone (1 / 1, v / v) mixed solution, n-hexane:acetone (volume ratio, 2:3) mixed solution, n-hexane : acetone (volume ratio, 3:2) mixture, n-hexane: dichloromethane (volume ratio, 2:3) mixture and n-hexane: water (volume ratio, 2:3) mixture, microwave extraction at 110 ° C 20min, cooled to r...

Embodiment 3

[0074] This embodiment focuses on the pretreatment technology of 13 kinds of brominated flame retardants in poultry eggs, and the proportion of acidic silica gel is selected according to the fat content of the actual sample. Since the fat content of duck eggs is relatively higher than that of chicken eggs, the purification effect is improved and the amount of acidic silica gel is increased.

[0075] Step 1: Buy domestic duck eggs from a farmer’s home in an electronic dismantling concentration area, put them in an ice box and take them back to the laboratory, remove the egg shells, put them in a stainless steel bowl and use a glass rod to stir the egg white and egg yolk evenly, and freeze them at -20°C. Solid state, use a freeze dryer to freeze-dry, accurately weigh 2.0g of the sample, add an appropriate amount of anhydrous sodium sulfate, and grind evenly. Completely transfer to a microwave extraction tube, add 30ml of n-hexane / acetone (50 / 50, v / v) mixture, extract by microwav...

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Abstract

The invention relates to a detection method for content of brominated flame retardants (BFRs) in food. The method comprises the following steps of carrying out microwave-assisted extraction on the food, carrying out centrifugation, collecting supernate, and concentrating the supernate to obtain extract solution; passing a composite column by the extract solution, carrying out elution and collecting eluent; employing a capillary column of which column length is 8-15m, inner diameter is 0.1-0.25mm and liquid film thickness 0.10-0.25mum, detecting the eluent through combination of a GC-NCI-MS selected ion mode (SIM), and carrying out quantitative calculation to obtain the content of the brominated flame retardants through adoption of an external standard method. Compared with a conventional method, the method has the advantages that the method is characterized by simplicity, speediness, accuracy and efficiency, and the lowest detection limit and a recovery rate of a sample and repeated test results satisfy detection for residual quantity of various BFRs in the food such as eggs.

Description

technical field [0001] The invention belongs to the fields of analytical chemistry and food safety, and in particular relates to a method for detecting the content of brominated flame retardants in food. Background technique [0002] Brominated flame retardants (BFRs) are a class of bromine-containing organic flame retardants, which are widely used in electronic appliances, plastics, foams, furniture, decoration and fiber due to their small addition amount and good flame retardant effect. products, etc. Polybrominated diphenyl ethers (PBDEs) are a class of commonly used additive brominated flame retardants. Commonly used commercial products mainly include pentabromodiphenyl ether (penta-BDE), octabromodiphenyl ether (octa-BDE) and decabromobiphenyl Ether (deca-BDE). Due to the persistence, bioaccumulation and possible biotoxicity of PBDEs in the environment, and even carcinogenicity, the commercial products of pentabromodiphenyl ether, octabromodiphenyl ether and decabromo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/062G01N2030/884
Inventor 王俊霞顾海东闫广礼赵佳平张占恩林匡飞韩艳娜马一飞刘缘廖方新刘姗姗李涵颖杨静文邹旭晴王婷刘一帆刘明月岑松岭胡韦高仕谦沈晓芳张磊杨光冠刘婷婷
Owner SUZHOU UNIV OF SCI & TECH
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