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A solid-phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for the online determination of hydroxy polycyclic aromatic hydrocarbons in urine

A triple quadrupole and isotope dilution technology, which is applied in the field of solid phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method, can solve the problems of unfavorable human sample screening, cumbersome method process, and large amount of solvent, and achieve The effect of omitting the pretreatment steps, reducing the risk of exposure, and reducing the amount of solvent

Active Publication Date: 2022-08-02
GUANGDONG UNIV OF TECH
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Problems solved by technology

At present, many literatures have reported that different methods are applied to the analysis of OH-PAHs in urine. Most of these methods require some pretreatment of urine. -PAHs enrichment and purification, the process is cumbersome, the amount of solvent is large, time-consuming and inefficient, and it is not conducive to large-scale screening of human samples

Method used

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  • A solid-phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for the online determination of hydroxy polycyclic aromatic hydrocarbons in urine
  • A solid-phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for the online determination of hydroxy polycyclic aromatic hydrocarbons in urine
  • A solid-phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for the online determination of hydroxy polycyclic aromatic hydrocarbons in urine

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Experimental program
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Embodiment 1

[0031] 1. Take 500μL of urine sample into a 1.5mL microcentrifuge tube, add OH-PAHs isotope internal standard (25ng 2-OH-Nap-d 7 , 10ng 2-OH-Flu-d 9 , 5ng 1-OH-Pyr-d 9 , 5ng 13 C 6 -3-OH-Phe, 5ng 3-OH-Bap-d 11 ) Add 5 μL β-glucuronidase-arylsulfatase and mix well, enzymolysis for 12 h on a constant temperature shaker at 37°C, add 500 μL acetonitrile to precipitate protein after enzymatic hydrolysis, vortex and mix for 1 min, and then perform high-speed refrigerated centrifugation (12000 rpm). , 10min, 4°C), after centrifugation, the supernatant was taken for injection.

[0032] 2. The model of online solid phase extraction-liquid chromatography-triple quadrupole mass spectrometry (LC-MS / MS) is Agilent 1260-6470 series. When automatic valve switching is used for online solid phase extraction, the six-port valve connects the 1 and 6 positions ( figure 1 Position 1), the injection volume is 500 μL; the online solid phase extraction enrichment column Eclipse Plus C18 column ...

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Abstract

The invention belongs to the technical field of organic pollutant analysis, and discloses a solid phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for online determination of hydroxy polycyclic aromatic hydrocarbons in urine. After labeling, β-glucuronidase-aryl sulfatase was added, and enzymolysis was carried out on a constant temperature shaker. After enzymolysis, an organic solvent was added to precipitate the protein, refrigerated and centrifuged, and the centrifuged supernatant was transferred, and online through automatic valve switching. Solid phase extraction followed by quantitative determination by liquid chromatography triple quadrupole mass spectrometry. After data processing and quantitative calculation, the content of hydroxy polycyclic aromatic hydrocarbons in urine was obtained. The invention realizes rapid and accurate detection of hydroxy polycyclic aromatic hydrocarbon metabolites in human urine, and provides an effective method and means for human exposure health risk assessment of polycyclic aromatic hydrocarbons.

Description

technical field [0001] The invention belongs to the technical field of organic pollutant analysis, and more particularly relates to a solid phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for online determination of hydroxy polycyclic aromatic hydrocarbons in urine. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs) are ubiquitous pollutants in the environment, mainly derived from the incomplete combustion of fossil fuels. PAHs can enter the human body through atmospheric respiration, dietary intake and skin absorption. Existing studies have clearly pointed out that PAHs have carcinogenic, teratogenic and mutagenic effects, and human lung cancer and other cancers are closely related to the exposure of PAHs. The half-life of PAHs in the human body is about a few hours. The PAHs absorbed by the human body can be metabolized and detoxified by the liver and other organs to form hydroxy polycyclic aromatic hyd...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/86
CPCG01N30/02G01N30/06G01N30/08G01N30/8675G01N2030/045G01N2030/062G01N2030/065
Inventor 马盛韬余应新李桂英安太成
Owner GUANGDONG UNIV OF TECH
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