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A multi-channel mass spectrometry derivatization reagent for detecting hydroxy polycyclic aromatic hydrocarbons and its preparation method and application

A technology for derivatizing reagents and polycyclic aromatic hydrocarbons, which is applied in the field of multi-channel mass spectrometry derivatizing reagents for detecting hydroxy polycyclic aromatic hydrocarbons and its preparation and application. It can solve the problems of expensive internal standard compounds, long derivatization time, and low analysis throughput. The method has good applicability, simple operation and high analytical throughput

Active Publication Date: 2022-03-25
QUFU NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Chinese patent (CN103175920A) discloses a kind of utilization N, O-bistrimethylsilylacetamide as derivatization reagent, through gas chromatography-mass spectrometry instrument to 1-hydroxy phenanthrene, 2-hydroxy phenanthrene, 3-hydroxy phenanthrene, 4-hydroxy phenanthrene, Hydroxyphenanthrene, 9-hydroxyphenanthrene, 1-hydroxypyrene, 3-hydroxybenzo[a]pyrene and 7-hydroxybenzo[a]pyrene detection method using 2-hydroxyphenanthrene-d 9 , 1-hydroxypyrene-d 9 and 3-hydroxybenzo[a]pyrene-d 11 Three deuterated compounds are used as internal standards, the derivation time is long, the sensitivity is low, and the internal standard compounds are expensive and difficult to purchase; Fluorene, 2-hydroxyphenanthrene, 3-hydroxyphenanthrene, 4-hydroxyphenanthrene and 1-hydroxypyrene are subjected to dispersion liquid-liquid extraction-floating droplet solidification method enrichment, combined with high performance liquid chromatography-fluorescence detection method for analysis and detection, which is time-consuming , low sensitivity, low throughput

Method used

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  • A multi-channel mass spectrometry derivatization reagent for detecting hydroxy polycyclic aromatic hydrocarbons and its preparation method and application
  • A multi-channel mass spectrometry derivatization reagent for detecting hydroxy polycyclic aromatic hydrocarbons and its preparation method and application
  • A multi-channel mass spectrometry derivatization reagent for detecting hydroxy polycyclic aromatic hydrocarbons and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0049] Chromatographic separation and mass spectrometry qualitative and quantitative analysis of 7 hydroxy polycyclic aromatic hydrocarbons:

[0050] Seven kinds of hydroxy PAH standard substances (purchased from Sigma, J&K and Aladdin Reagent Company) were prepared in acetonitrile to obtain a concentration of 1.0 × 10 -2 mol / L hydroxy polycyclic aromatic hydrocarbon standard solution. We centrifuged the analyte-free urine at high speed to remove impurities, added acetonitrile (1:3, v / v) to the analyte-free plasma, centrifuged for 5 minutes (12000rpm), separated the supernatant for use, and processed Unanalyzed urine and plasma were mixed in the same proportion as a blank matrix. Take 0.2 mL from each single-standard stock solution and dilute to 10 mL with a blank matrix to obtain a mixed-standard stock solution of hydroxy-PAHs. 4'-(N,N-dialkyl)-1-piperazinyl-6-carbonyl chloride-piperidic acid was dissolved in acetonitrile to obtain 1.0×10 -3 mol / L derivative reagent solution...

Embodiment 2

[0057] The detection and analysis of free hydroxy polycyclic aromatic hydrocarbons in urine includes the following steps:

[0058] Take 500 μL of urine from smokers or non-smokers and centrifuge at high speed to remove impurities, then take 9 parts of 50 μL urine samples and place them in 1.5 mL centrifuge tubes, and take another 50 μL standard mixed solution (1.0×10 -5 mol / L) in a 1.5mL centrifuge tube, add 250μL NaHCO 3 -Na 2 CO 3 (pH 9.8) buffer solution, vortex shaker for 15s, add 550 μL of other 9 kinds of SIMTs (SIMT-332 / 338 / 349 / 351 / 354 / 360 / 363 / 374 / 377) solution, SIMT-346 solution, Seal and react at 40°C for 4.5 minutes. Then the SIMT-346-labeled standard derivatization product solution (internal standard solution) and other 9 kinds of derivatization reagent-labeled urine sample derivatization product solutions were mixed in equal volumes in a 1.0mL test tube (derivatization product mixed solution), and then used for MDSPE program.

[0059] 7 mg of adsorbent (Fe 3 ...

Embodiment 3

[0061] The detection of free hydroxy polycyclic aromatic hydrocarbons in plasma includes the following steps:

[0062] Take 200 μL of plasma from smokers or non-smokers, add 100 μL of acetonitrile, centrifuge at high speed for 5 minutes (12000 rpm) and separate the supernatant for use. Take 9 parts of 20μL plasma samples and place them in 1.5mL centrifuge tubes, and take another 20μL standard mixed solution (1.0×10 -5 mol / L) in a 1.5mL centrifuge tube, add 100μL NaHCO 3 -Na 2 CO 3 (pH 9.0) buffer solution, vortexed for 15s, respectively added 150 μL other 9 kinds of SIMTs (SIMT-332 / 338 / 349 / 351 / 354 / 360 / 363 / 374 / 377) solution, SIMT-346 solution, Seal and react at 40°C for 6 minutes. Then the SIMT-346-labeled standard derivatization product solution (internal standard solution) and other 9 kinds of derivatization reagent-labeled plasma sample derivatization product solutions were mixed in equal volumes in a 1.0mL test tube (derivatization product mixed solution), and then used...

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Abstract

The invention belongs to the technical field of analytical chemistry, and in particular relates to a multi-channel mass spectrometry derivatization reagent for detecting hydroxyl polycyclic aromatic hydrocarbons and its preparation method and application, in particular to a method using 4'-(N,N-dialkyl)-1 ‑Piperazinyl‑6‑carbonyl chloride‑piperidic acid as a derivatization reagent, multi-channel stable isotope labeling derivatization-magnetic dispersion solid phase extraction combined with ultra-high performance liquid chromatography triple quadrupole mass spectrometry for the analysis of a variety of free hydroxyl polycyclic aromatic hydrocarbons method. The structural formula of the derivative reagent is:. The invention can realize simultaneous detection of various hydroxy polycyclic aromatic hydrocarbons in nine actual samples with one injection. Quantification by the internal standard method can obtain the content of hydroxy polycyclic aromatic hydrocarbons in the actual sample. This method has the advantages of high throughput, rapidity, high sensitivity, high accuracy and high selectivity. This method provides an accurate and reliable technical means for assessing human PAH exposure levels.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and specifically relates to a multi-channel mass spectrometry derivatization reagent for detecting hydroxyl polycyclic aromatic hydrocarbons and its preparation method and application, especially to a method using 4'-(N,N-dialkyl)-1 -Piperazinyl-6-carbonyl chloride-piperidic acid as a derivatization reagent, multi-channel stable isotope labeling derivatization-magnetic dispersion solid-phase extraction combined with ultra-high performance liquid chromatography triple quadrupole mass spectrometry for the analysis of various free hydroxyl polycyclic aromatic hydrocarbons method. Background technique [0002] Exposure to polycyclic aromatic hydrocarbons (PAHs) poses a serious threat to human health, such as lung cancer, diabetes, and cardiovascular and cerebrovascular diseases. At the same time, pregnant women exposed to high concentrations of PAHs can cause miscarriage, premature birth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/04G01N30/02G01N30/06G01N30/32G01N30/34G01N30/72
CPCC07D471/04G01N30/02G01N30/06G01N30/32G01N30/34G01N30/72C07B2200/05G01N2030/062G01N2030/324
Inventor 朱树芸孙鲁平赵先恩
Owner QUFU NORMAL UNIV
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