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Detecting method for multiple kinds of poly brominated diphenyl ethers in aquatic product

A technology with multiple polybrominated and detection methods, applied in the field of determination of polybrominated diphenyl ethers, can solve the problems of large amount of solvent consumption, difficult to achieve, long peak time, etc., to shorten the detection cycle, reduce the detection cost and short detection time Effect

Inactive Publication Date: 2013-08-07
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0019] However, in prior art reports, there are still some defects: 1. can only be detected for one or several specific PBDEs, and the number of homologues of PBDEs is large (up to 209 kinds), they cannot detect more simultaneously Many kinds of PBDEs; 2. Part of the pretreatment process is complex, time-consuming, requires high equipment and consumes a large amount of solvent; 3. Some analysis and detection processes cannot separate multiple PBDEs at the same time and the peak time is very long, and some can Simultaneous separation of multiple PBDEs can be achieved but the detection of residue levels cannot be achieved, especially it is difficult to simultaneously detect BDE209 (the response in the detection instrument is relatively low) and other PBDEs, so different methods have to be used for detection
However, so far, there is no complete and reliable patent for the multi-residue rapid detection of PBDEs in aquatic products, so the present invention emerges at the historic moment

Method used

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  • Detecting method for multiple kinds of poly brominated diphenyl ethers in aquatic product
  • Detecting method for multiple kinds of poly brominated diphenyl ethers in aquatic product
  • Detecting method for multiple kinds of poly brominated diphenyl ethers in aquatic product

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Effect test

Embodiment 1

[0063] Because the 11 kinds of PBDEs homologues involved in the present invention all have differences in their respective boiling points, polarity and adsorption properties, resulting in different adsorption or dissolution capabilities of each component in the fixed phase sample, that is, each component is in the stationary phase and The partition coefficients between mobile phases are different, so their peak eluting times will be different. In order to ensure that each target pollutant has a good separation effect and chromatographic peak shape, by adopting the detection method of the present invention, not only the separation of 11 kinds of PBDEs is well realized, but also the separation degree of each peak is large, the peak shape is sharp, and the symmetry is good . After many experiments and repeated identification, the reference retention time of each standard substance under the operating conditions of the present invention is obtained, which is specifically shown in ...

Embodiment 2

[0072] Prepare 11 kinds of PBDEs with n-hexane to prepare a single standard solution with a certain concentration, and then take a certain amount of each, and mix them to prepare a series of 11 kinds of PBDEs standard working solutions: the serial concentrations of BDE206 and 208 are 0.1, 0.2, 0.4 respectively , 1.0, 2.0, 4.0, 10.0, 20.0, 40.0, 100.0, 200.0 and 2000.0ng / mL, the serial concentrations of BDE209 are 0.5, 1.0, 2.0, 5.0, 10.0, 20.0, 50.0, 100.0, 200.0, 500.0, 1000.0 and 10000.0ng / mL, the serial concentrations of other PBDEs were 0.05, 0.1, 0.2, 0.5, 1.0, 2.0, 5.0, 10.0, 20.0, 50.0, 100.0 and 1000.0ng / mL. According to the above-mentioned instrument detection conditions sample introduction detection of embodiment 1, carry out linear regression analysis to the mass concentration x (ng / mL) of standard working solution with the peak area y of each component respectively, draw the linear regression equation, correlation of each standard substance Coefficients and method ...

Embodiment 3

[0077] The recovery rate experiments of crucian carp and herring were carried out to investigate the applicability of the established detection method.

[0078] Weigh 1.00g of crucian carp and herring muscle samples with no PBDEs detected, and add 200ng of BDE-15, BDE-28, BDE-47, BDE-100, BDE-99, BDE-154, BDE -153 and BDE-183 standard samples, BDE-208 and BDE-206 standard samples were added in an amount of 400ng, and BDE-209 standard samples were added in an amount of 2000ng. The spiked amounts of PBDEs in these three groups were equivalent to 200ng / g, 400ng / g and 2000ng / g, respectively.

[0079] Weigh 1.00 g of crucian carp and herring muscle samples without PBDEs detected, and add 100 ng of BDE-15, BDE-28, BDE-47, BDE-100, BDE-99, BDE-154, BDE -153 and BDE-183 standard samples, BDE-208 and BDE-206 standard samples were added in an amount of 200ng, and BDE-209 standard samples were added in an amount of 1000ng. The spiked amounts of PBDEs in these three groups were equivale...

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Abstract

The invention relates to a detecting method for multiple kinds of poly brominated diphenyl ethers in an aquatic product. The detecting method comprises the steps of carrying out extracting, degreasing, silicagel column purifying and concentrating on an aquatic product sample, and analyzing and detecting the aquatic product sample through gas chromatography-negative chemical ionization mass spectrometry. By adopting the treatment measures and proper technique parameters, the method is capable of simply, quickly and accurately measuring the contents of as much as 11 kinds of poly brominated diphenyl ethers in the aquatic product at the same time, and the method has the advantages of high detecting sensitivity, good stability, accurate result, and the like, thereby providing a reliable and quick detecting method for qualitatively and quantitatively detecting the residual poly brominated diphenyl ethers in the aquatic product and monitoring food safety.

Description

technical field [0001] The invention provides a detection method for biologically toxic and harmful substances, in particular a method for determining up to eleven kinds of polybrominated diphenyl ethers in aquatic products, and belongs to the field of safety detection of harmful substance residues in agricultural by-products. Background technique [0002] Polybrominated diphenyl ethers (Polybrominated Diphenyl Ethers, PBDEs) are a class of brominated flame retardants. Due to their excellent flame retardancy, good thermal stability, small addition, and low price, they are widely used in the electronics industry, foam plastics, It has been widely used in textiles, building materials, home appliances, home decoration, chemical products, petroleum, mining and other fields, and the annual demand is huge. [0003] Polybrominated diphenyl ethers have up to 209 homologues due to changes in the number and position of bromine, mainly including: 4,4'-dibromodiphenyl ether (BDE-15), 2,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/14G01N30/32
Inventor 张卫陈雷刘扣陈琳林匡飞郭杰周啸宇黄凯周鹏徐峰傅晓旭邓晶晶刘洋成张荣李靖
Owner EAST CHINA UNIV OF SCI & TECH
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