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A method for detecting tetrabromobisphenol A in waters by gas chromatography-mass spectrometry

A technology of gas chromatography mass spectrometry and tetrabromobisphenol, which is applied in the field of environmental or aquatic product detection, can solve the problems of migration to remote or even polar regions, interference of organic pollutant detection results, pollution of brominated flame retardants, etc., and achieves superior performance , high accuracy and high sensitivity

Active Publication Date: 2017-07-14
CHINA CERTIFICATION & INSPECTION GRP HUBEI CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, brominated flame retardants released from flame retardant materials will remain in environmental media such as soil, water, sediment and sediment, as well as biological media such as human body, animal and plant bodies for decades or even longer, and the residual Brominated flame retardants can migrate to remote or even polar regions through the atmospheric "global distillation effect" and "grasshopper jump effect", causing global brominated flame retardant pollution
[0003] There are more and more types of organic pollutants in the environment and aquatic products, and the matrix in which such organic pollutants are located is also very complex. If the impurities are not treated, they will greatly interfere with the subsequent detection results of organic pollutants. affect the results of the test

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Measure 500mL water sample, put the water sample into a 2L separatory funnel, add tetrabromobisphenol A and isotope internal standard solution (MTBBPA), mix the solution evenly and equilibrate for 1~2h.

[0024] For water extraction, take 500mL water sample in a separatory funnel, extract with 150mL chloroform for 3 times, combine the extracts into a concentration bottle, concentrate at a temperature of 40°C, concentrate to about 1mL, then transfer the concentrate to a nitrogen blowpipe, Then use 5mL of the mixed extract solution to rinse the concentrated bottle twice, put the washing solution into the nitrogen blowing pipe, put the nitrogen blowing pipe on the nitrogen blowing instrument, the nitrogen blowing temperature is 40°C, blow the nitrogen to about 0.5mL, and then add 5mL Nitrogen blowing with n-hexane was repeated 3 times, and finally concentrated to 1.0 mL, followed by gel chromatography purification.

[0025] 2. Weigh 40g of gel, dissolve it in 150mL acet...

Embodiment 2

[0033] 1. Weigh 1.0g of fish blood or 5.0g of bottom mud, add tetrabromobisphenol A and isotope internal standard solution (MTBBPA) into it, put the bottom mud or fish blood samples into the refrigerator to freeze (-18°C), and wait until After the freezing is complete, put the frozen bottom mud or fish blood into the freeze dryer, the freeze dryer pre-freezing temperature is -20℃~-40℃, the freeze drying temperature is -30℃~-50℃, the fish blood or bottom mud, Add diatomaceous earth to the fish blood (fish blood: diatomaceous earth = 1:1), add diatomaceous earth to the bottom mud (bottom mud: diatomaceous earth = 5:1), mix well, and put the sample into the cable after mixing. Extract the filter cartridge and place the Soxhlet extraction device. Inject 50mL of n-hexane and acetone (1:1) mixed extract, soak the Soxhlet filter cartridge and place it overnight. Add 50 mL of n-hexane and acetone (1:1) mixed extract solution to a round bottom flask, extract in a water bath at 60°C fo...

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Abstract

The invention provides a method for detecting tetrabromobisphenol A in waters through gas chromatography-mass spectrometry. The method comprises the following steps: (1) detected sample pretreatment: selecting a water body or sediment in the waters or blood of fish living in the waters as the detected sample; (2) gel column preparation: weighing gel, firstly soaking the gel with mixed eluent overnight and then pouring the gel into a chromatographic column, wherein the mixed eluent is a mixed solution of n-hexane and acetone; (3) sample purification; (4) derivatization and quantification; (5) analysis by gas chromatograph-mass spectrometer (GC-MS): analyzing a sample solution obtained in the step (4) by adopting the GC-MS to detect the content of tetrabromobisphenol A in the sample solution. The method provided by the invention can achieve the effect of reducing interference of the impurities in the sample and the exogenous impurities, thus achieving accurate quantification of tetrabromobisphenol A by the GC-MS. The method has the advantages of simplicity in operation, good repeatability and high accuracy.

Description

technical field [0001] The invention relates to a preparation method of a tetrabromobisphenol A gel chromatographic column detected by a gas chromatography-mass spectrometer and a detection method of tetrabromobisphenol A, which belong to the technical field of environment or aquatic product detection. Background technique [0002] At present, with the enhancement of people's awareness of fire prevention and the improvement of fire safety standards, the application of flame retardant materials is becoming more and more extensive. Brominated flame retardants (BFRs) have become the organic flame retardants with the largest production and consumption in the world due to their mature production process, stable properties, and good flame retardant performance. Many compounds in brominated flame retardants are persistent, lipophilic, and bioaccumulative. Therefore, brominated flame retardants released from flame retardant materials will remain in environmental media such as soil,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/14
CPCG01N30/14
Inventor 胡德聪胡小钟王惠张华吴斌林长军
Owner CHINA CERTIFICATION & INSPECTION GRP HUBEI CO LTD
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