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Method for SPME (solid phase micro-extraction)-MS (mass spectrometry) combined online enrichment detection of nicotine compounds in tobaccos

A technology for nicotinic compounds and compounds, which is applied in the field of solid-phase microextraction-mass spectrometry online enrichment detection of nicotinic compounds in tobacco, which can solve the problems of affecting the accuracy of inspection results, affecting the performance of mass spectrometry analysis, and the content of target compounds is low. problems, achieve good enrichment performance and selectivity, simplify the pretreatment process, and achieve the effect of small sample volume

Active Publication Date: 2018-11-16
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When ESI-MS encounters the actual sample, due to the complex composition of the actual sample, the low content of the target compound, and matrix problems, it may also cause problems such as contamination and blockage of the mass spectrometer, which will affect the accuracy of the inspection results or affect the analytical performance of the mass spectrometer.

Method used

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  • Method for SPME (solid phase micro-extraction)-MS (mass spectrometry) combined online enrichment detection of nicotine compounds in tobaccos
  • Method for SPME (solid phase micro-extraction)-MS (mass spectrometry) combined online enrichment detection of nicotine compounds in tobaccos
  • Method for SPME (solid phase micro-extraction)-MS (mass spectrometry) combined online enrichment detection of nicotine compounds in tobaccos

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] First use methanol for 15min, water for 15min, 0.1mol L -1 HCl solution for 30 minutes to wash the whole empty capillary column (with an inner diameter of 150 μm) to remove organic and inorganic impurities remaining on the inner wall of the capillary. Next, feed secondary water until the solution that flows out is basically neutral. Then use 0.1mol L -1 The NaOH solution activates the inner wall of the capillary monolithic column for about 3 hours, then passes through secondary water again to neutrality, and finally passes through methanol for 30 minutes, and blows dry with nitrogen for 30 minutes.

[0031] A mixture of methanol:γ-MAPS=50:50 (v / v) was evenly injected into the activated capillary, and reacted for 24 hours to silanize the inner wall of the capillary. After the silanized capillary column is passed through methanol, the silane reagent is washed away. Blow dry with nitrogen.

[0032] Reaction monomer: NIPAAm (60mg); Cross-linking agent: DVB (80mg), MBAA ...

Embodiment 2

[0034] The poly(NIPAAm-co-DVB-co-MBAA) polymer monolithic column is used in combination with API-MS, and the connection method is as follows figure 2 shown. Two micro-sampling syringe pumps A 1 and B 2 are respectively used as the driving force for the analysis sample and the elution solvent, passing through the PEEK tube 3, the tee tube 4 and the poly(NIPAAm-co-DVB-co-MBAA) polymer monolithic column 5 to link up. Then through a two-way tube 6 and a PEEK tube 3, it is connected to the ESI of the vacuum chamber in the vacuum electrospray-mass spectrometer detector API-M7S. The analyte undergoes sample extraction, elution and other procedures, and finally enters the mass spectrometer for analysis.

[0035] After condition optimization, the optimal conditions are: the content of acetonitrile (99%, v / v) in the sample, the extraction flow rate (30μLmin -1 ), formic acid concentration (0.01%, v / v), water concentration, elution flow rate, elution time, adopt the following enrichm...

Embodiment 3

[0038] Sample solution: 300 μL; solvent is water: ACN=99:1 (v / v); injection flow rate: 30 μL min -1 ; Extraction time: 10min; Elution solution: ACN: 0.01% formic acid aqueous solution = 95:5 (v / v); Elution flow rate: 10 μ L min -1 ; Elution time: under the condition of 10 minutes, the method is used to detect and analyze six kinds of nicotine compounds in tobacco samples, and the detection range is 1-100 ng / mL, and the detection parameters are shown in Table 1.

[0039] Table 1 Analytical parameters obtained by analyzing six kinds of nicotine compounds by solid-phase microextraction-mass spectrometry in tube

[0040]

[0041] Note: R2 correlation coefficient; RSD relative standard deviation.

[0042] The results in Table 1 show that the detection limit can reach 0.140~0.644ng·mL -1 , the lowest detection amount can reach 1.99~4.06ng·mL -1 , the deviation in the same day is 5.89-6.43%, and the deviation in different days is 10.3-12.6%.

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Abstract

The invention discloses a method for SPME (solid phase micro-extraction)-MS (mass spectrometry) combined online enrichment detection of nicotine compounds in tobaccos. By means of online combination of a Poly(DVB-co-NIPPAm-co-MBAA) polymerized monolithic micro-extraction column and API-MS (atmospheric pressure ionization mass spectrometry), online enrichment detection of the nicotine compounds inthe tobaccos is realized. By means of online combination of the monolithic micro-extraction column and the API-MS and with application of noncovalent-bond interaction such as hydrogen bond, pi-pi bondand hydrophobicity of the surface of the monolithic micro-extraction column with the nicotine compounds, the method is applied to enrichment of harmful nicotine substances, and online analysis of thenicotine compounds can be realized. The method is simple, cheap and easy to operate, the multiple harmful nicotine components in tobaccos are rapidly extracted and enriched, detection sensitivity ofthe method is improved, matrix interference is reduced, and the high-efficient detection requirement for the nicotine compounds in tobaccos is met.

Description

technical field [0001] The invention belongs to the technical field of food detection, separation and analysis, and in particular relates to a solid-phase microextraction-mass spectrometry online enrichment detection method for nicotinic compounds in tobacco. Background technique [0002] Tobacco contains many chemical substances that are harmful to life and health, and these substances are the pathogenic factors of many diseases, such as: lung disease, cardiovascular disease, asthma, diabetes and cancer. Therefore, the existence of some components such as nicotine in tobacco is still very important to people's health. According to analysis, nicotine is a compound with high content and high toxicity in tobacco, which is also called nicotine. And the unique nitrosamine compounds in nicotine are a large class of compounds that affect health. Among them, the more common and more toxic ones include: 1-(4-nitrophenyl)piperazine (1-(4-Nitrophenyl)piperazine, referred to as NHK),...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/72
CPCG01N30/06G01N30/72G01N2030/062
Inventor 吴芳玲王亮杨淑童丁航宇储艳秋丁传凡
Owner FUDAN UNIV
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