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Method for determining contents of phosphodiester metabolites of organophosphorus esters (OPEs) in plasma

A technology of phosphodiester and metabolites, which is applied in the field of determination of phosphodiester metabolites of OPEs in plasma, can solve the problems of poor anti-interference ability and insufficient sensitivity, and achieve strong anti-interference ability, high detection sensitivity, and shorten the extraction time. the effect of time

Active Publication Date: 2020-02-18
NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem solved by the present invention is: there is certain limitation in existing detection method, sensitivity is not high enough, anti-interference ability is poor etc., provides a kind of determination diethyl phosphate, di-n-butyl phosphate and di-n-butyl phosphate in sediment sample The method of diphenyl phosphate, which has a low detection limit and good stability, can basically meet the detection requirements of diethyl phosphate, di-n-butyl phosphate and diphenyl phosphate in blood samples

Method used

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  • Method for determining contents of phosphodiester metabolites of organophosphorus esters (OPEs) in plasma
  • Method for determining contents of phosphodiester metabolites of organophosphorus esters (OPEs) in plasma
  • Method for determining contents of phosphodiester metabolites of organophosphorus esters (OPEs) in plasma

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A method for measuring the content of phosphodiester metabolites of OPEs in plasma, comprising the following steps:

[0036] S1: Modification of plasma:

[0037] Take 3mL of plasma and put it into a centrifuge tube, add 3mL of formic acid, mix well and equilibrate for 3 hours, add 9mL extract solution (n-hexane 15ng / ml) and shake and extract for 4 hours;

[0038] S2: Sample pretreatment:

[0039] Centrifuge the sample, take out the upper organic phase, add the mixed phase of plasma, water and formic acid in the lower layer to 9mL extract solution (n-hexane), shake and extract for 30min, repeat this step once, combine the organic phase, and pass through anhydrous Na 2 SO 4 After removing the water, evaporate to dryness by rotary evaporation, and replace the solvent with 5mL acetonitrile;

[0040] Fill the glass column sequentially from bottom to top with 100mg N-propylethylenediamine solid-phase adsorbent PSA, 20mg graphitized carbon black GCB, 4g anhydrous Na 2 SO ...

Embodiment 2

[0054] A method for measuring the content of phosphodiester metabolites of OPEs in plasma, comprising the following steps:

[0055] S1: Modification of plasma:

[0056] Take 3mL of plasma and put it into a centrifuge tube, add 3mL of formic acid, mix well and equilibrate for 3 hours, add 9mL extract solution (ethyl acetate 20ng / ml) and shake and extract for 5 hours;

[0057] S2: Sample pretreatment:

[0058] Centrifuge the sample, take out the upper organic phase, add the mixed phase of plasma, water and formic acid in the lower layer to 9mL extract solution (ethyl acetate), shake and extract for 30min, repeat this step once, combine the organic phase, and pass through anhydrous Na 2 SO 4 After removing the water, evaporate to dryness by rotary evaporation, and replace the solvent with 5mL acetonitrile;

[0059] Fill the glass column sequentially from bottom to top with 100mg N-propylethylenediamine solid-phase adsorbent PSA, 20mg graphitized carbon black GCB, 4g anhydrous ...

Embodiment 3

[0073] A method for measuring the content of phosphodiester metabolites of OPEs in plasma, comprising the following steps:

[0074] S1: Modification of plasma:

[0075] Take 3mL of plasma and add it to a centrifuge tube, add 3mL of formic acid, mix well and equilibrate for 3 hours, add 9mL of extract solution (mixed with n-hexane 25ng / ml and ethyl acetate 25ng / ml in equal volume ratio) and shake for 6 hours;

[0076] S2: Sample pretreatment:

[0077] Centrifuge the sample, take out the upper organic phase, add the mixed phase of plasma, water and formic acid in the lower layer to 9mL extract solution (n-hexane and ethyl acetate are mixed in equal volume ratio), shake and extract for 30min, repeat this step once, combine the organic phase, Anhydrous Na 2 SO 4 After removing the water, evaporate to dryness by rotary evaporation, and replace the solvent with 5mL acetonitrile;

[0078] Fill the glass column sequentially from bottom to top with 100mg N-propylethylenediamine sol...

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Abstract

The invention relates to the technical field of determination of contaminants in plasma, particularly to a method for determining the contents of phosphodiester metabolites of organophosphorus esters(OPEs) in the plasma. The method is characterized in that the high-performance liquid chromatography-ion trap-triple quadrupole mass spectrometry technology is combined with liquid-liquid extraction and extraction through a self-made solid-phase column for detection of the contents of diethyl phosphate, dibutyl phosphate and diphenyl phosphate in the plasma; and plasma samples are purified throughthe liquid-liquid extraction and the solid-phase extraction, analysis is carried out through an ion monitoring mode of a high-performance liquid chromatograph-mass spectrometer MRM, and quantification is carried out through the external standard method. The method provided by the invention has the advantages of low detection limit, high stability, high recovery rate and high detection sensitivity, is applicable to the determination of the contents of the diethyl phosphate, the dibutyl phosphate and the diphenyl phosphate in the human plasma, and can meet detection requirements for residues oftarget substances in the human plasma.

Description

technical field [0001] The invention relates to the technical field of biological sample organic pollutant detection, in particular to a method for measuring the content of phosphodiester metabolites of OPEs in blood plasma. Background technique [0002] With the prohibition of organochlorine and organobromine flame retardants such as polychlorinated biphenyls and polybrominated diphenyl ethers in the Stockholm Convention on Persistent Organic Pollutants, organophosphate esters (OPEs) flame retardants have been used as alternative flame retardants in recent years. have been widely applied. Since OPEs are usually added to samples in physical form rather than chemical form, they are easily released into the environment during the production, transportation and use of products. At present, the existence of OPEs has been detected in many environmental matrices including air, water and soil, especially the indoor environmental dust is an important "sink" of OPEs, and OPEs in env...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 张芹宋宁慧张圣虎唐夫凯刘爱萍卜元卿王博李栋王艺璇
Owner NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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