Solid-phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for online determination of hydroxyl polycyclic aromatic hydrocarbon 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 Reduced solvent usage and pretreatment time, reduced exposure risk, and reduced solvent usage

Active Publication Date: 2020-11-24
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 en

Method used

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  • Solid-phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for online determination of hydroxyl polycyclic aromatic hydrocarbon in urine
  • Solid-phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for online determination of hydroxyl polycyclic aromatic hydrocarbon in urine
  • Solid-phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for online determination of hydroxyl polycyclic aromatic hydrocarbon in urine

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Embodiment 1

[0031] 1. Take 500 μL urine sample and put it 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 of β-glucuronidase-arylsulfatase and mix well, enzymolyze on a constant temperature shaker at 37°C for 12 hours, add 500 μL of acetonitrile to precipitate protein after enzymolysis, vortex and mix for 1 min, and then carry out high-speed refrigerated centrifugation (12000rpm , 10min, 4°C), after centrifugation, the supernatant was taken for injection.

[0032] 2. The model of the online solid phase extraction-liquid chromatography-triple quadrupole mass spectrometry (LC-MS / MS) is Agilent 1260-6470 series. When using automatic valve switching for online solid phase extraction, the six-way valve connects 1 and 6 ( figure 1 Position 1), the injection volume is 500μL; the online solid phase extraction enrichment column Eclipse Plus C18 column (4.6×3...

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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 foronline determination of hydroxyl polycyclic aromatic hydrocarbon in urine. The method comprises the following steps: adding an isotope internal standard into urine, and then adding beta-glucuronidase-aryl sulfatase; carrying out enzymolysis on a constant-temperature shaking table, adding an organic solvent to precipitate protein after enzymolysis, carrying out refrigerated centrifugation, transferring the centrifuged supernatant, carrying out online solid-phase extraction through automatic valve switching, and then carrying out quantitative determination through liquid chromatography triple quadrupole mass spectrometry; and carrying out data processing and quantitative calculation to obtain the content of the hydroxyl polycyclic aromatic hydrocarbon in the urine. According to the invention, rapid and accurate detection of hydroxyl polycyclic aromatic hydrocarbon metabolites in human urine is realized, and an effective method is provided for human exposure health risk assessment of polycyclic aromatic hydrocarbon.

Description

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

Claims

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Application Information

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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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