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Gas chromatography-tandem quadrupole mass spectrometry analysis method of soil / sediment organophosphate flame retardant

A series of quadrupole, organic phosphate technology, applied in the field of analytical chemistry, can solve the problems of complex operation procedures, large solvent consumption, low sensitivity, etc. Effect

Inactive Publication Date: 2015-11-18
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The invention provides a time-saving, labor-saving, efficient and accurate detection of organic phosphate in solid-phase environmental media such as soil / sediment, aiming at large solvent consumption, long time, complicated operation procedures, serious matrix interference, and low sensitivity during the experiment. Analytical method

Method used

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  • Gas chromatography-tandem quadrupole mass spectrometry analysis method of soil / sediment organophosphate flame retardant
  • Gas chromatography-tandem quadrupole mass spectrometry analysis method of soil / sediment organophosphate flame retardant

Examples

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Embodiment 1

[0028] Using the present invention to analyze the organophosphate in the sediment of Tangxi River in Hefei City, take an appropriate amount of sediment to freeze-dry for 48 hours, use a grinder to grind, and pass through a 80-100 mesh sieve. Weigh three 2.0g sediment samples with an electronic balance, put them into three 30mL glass centrifuge tubes respectively, add 10ngTnBP-D27 to the samples, add 20mL acetone:n-hexane (V:V=1:1) extraction solvent, Seal the mouth of the centrifuge tube with aluminum foil, put it into an ultrasonic instrument and sonicate for 10 minutes, then centrifuge at 3000rpm for 10 minutes, separate the supernatant extract into a flat-bottomed flask; repeat the extraction once, and mix the extract twice. Concentrate the extract on a rotary evaporator and transfer it to a screw-top test tube, wash the wall of the bottle with 3 mL of n-hexane for 3 times, transfer the washing liquid to a screw-top test tube, and blow nitrogen to about 1 mL. Put the activa...

Embodiment 2

[0036] For the analysis of organophosphates in the sediments of the Shishili River in Hefei City, an appropriate amount of sediments was freeze-dried for 48 hours, ground by a grinder and passed through a sieve of 80-100 mesh. Weigh three 2.0g sediment samples with an electronic balance, put them into three 30mL glass centrifuge tubes respectively, add 10ngTnBP-D27 to the samples, add 20mL acetone:n-hexane (V:V=1:1) extraction solvent, Seal the mouth of the centrifuge tube with aluminum foil, put it into an ultrasonic instrument and sonicate for 10 minutes, then centrifuge at 3000rpm for 10 minutes, separate the supernatant extract into a flat-bottomed flask; repeat the extraction once, and mix the extract twice. Concentrate the extract on a rotary evaporator and transfer it to a screw-top test tube, wash the wall of the bottle with 3 mL of n-hexane for 3 times, transfer the washing liquid to a screw-top test tube, and blow nitrogen to about 1 mL. Put the activated copper into...

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Abstract

The present invention relates to an analysis method of soil / sediment organophosphate flame retardant, and belongs to quantitative analysis method of organic pollutants in the field of analytical chemistry. The method tests eight organophosphate in a soil / sediment solid-phase sample. The method is as below: freeze-drying, grinding and sieving the sample, storing the sample in a glass vial (4 DEG C); extracting by an oscillation and ultrasonic method; and purifying by Florisil column for pretreatment. The method is simple for sample pretreatment, and uses short time and less solvent; gas chromatography-tandem quadrupole mass spectrometer is used for qualitative and quantitative determination of eight organophosphates, and achieves good separation of all the target substances within 19 min. the object recovery is 80%-120% (except triethylphosphate of 72.9%), and the detection limit is 0.31-64.51ng / L; and the method has good precision and accuracy.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to a quantitative analysis method for organic pollutants. Specifically, it is a method of extracting organic phosphates in soil / sediment by vibration + ultrasound, purified by Florisil column, and qualitatively and quantitatively analyzing 8 kinds of organic phosphates by gas chromatography-tandem quadrupole mass spectrometry . Background technique [0002] Organophosphate esters (organophosphateesters, OPEs) are compounds formed by replacing the hydrogen on the phosphoric acid molecule with different hydrocarbon substituents (alkyl, chloroalkyl, aromatic). Due to the excellent flame retardant properties of OPEs and the gradual ban of polybrominated diphenyl ether flame retardants worldwide, the global production of OPEs has gradually increased. Studies at home and abroad have shown that OPEs are very stable, and alkyl and aryl OPEs have strong biological effects. Among them, tri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 张华胡晓辉刘世龙仇雁翎朱志良
Owner TONGJI UNIV
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