Phosphorus carpentine positive ion and gas-phase preparation and application thereof

A cation and gas-phase technology, applied in chemical instruments and methods, instruments, analytical materials, etc., can solve the problems of limited generation and separation methods of phosphocarbene cations, few studies on properties and activities, and achieve rapid qualitative and quantitative detection with simple methods Ease of operation, simple method and effect

Active Publication Date: 2018-01-30
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the research on carbocation and carbon carbene has gradually matured, but due to the limited production and separation methods of phosphorus carbene cation, there are still few studies on its properties and activities.

Method used

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  • Phosphorus carpentine positive ion and gas-phase preparation and application thereof
  • Phosphorus carpentine positive ion and gas-phase preparation and application thereof
  • Phosphorus carpentine positive ion and gas-phase preparation and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1 (gas-phase preparation method of diphenylphosphocarbene cation)

[0031] Adopt the mass spectrometry device of the gas-phase molecular-ion reaction disclosed in the Chinese patent application number 201510254326.1, the principle of the gas-phase preparation method of the diphenylphosphocarbene cation in Example 1 is as follows figure 1 shown;

[0032] (1) 1 mg of triphenylmethylphosphonium bromide was dissolved in 1ml of methanol, and the mass spectrum signal m / z 277 of triphenylmethylphosphorus cation could be detected in ESI-MS positive ion mode;

[0033] (2) The mass spectrum peak of m / z 277 was fragmented by collision-induced dissociation (CID) to obtain a fragment peak of m / z 185, which was diphenylphosphocarbene cation.

Embodiment 1 2

[0034] The gas phase preparation mass spectrogram of embodiment 1 diphenylphosphocarbene cation is as follows figure 2 As shown, the diphenylphosphocarbene cation obtained in the gas phase was characterized by high-resolution mass spectrometry, and the results are as follows: accurate molecular weight determination calculated for C 12 h 10 P + :185.0515,found:185.0507,relative error:-4.32ppm.

Embodiment 2

[0035] Embodiment 2 (the gas phase molecule-ion reaction of diphenylphosphocarbene cation)

[0036] After selective isolation of the diphenylphosphocarbene cation obtained in the MS / MS, the molecular reagents were introduced into the ion trap, and (a) acetonitrile, (b) formic acid, (c) acrylonitrile, (d) dichloromethane were selected. , (e) ethyl acetate, (f) n-butanol, (g) tert-butanol, (h) triethylamine, (i) benzene and (j) styrene total 10 kinds of reagents with diphenylphosphocarbene The cation reacts, and the partial pressure of the reaction gas is controlled at (0.4-0.6)x10-5 Torr, the control time is between 500ms and 1s, and clear response results can be obtained such as image 3 shown. These 10 kinds of molecular reagents can react with diphenylphosphocarbene cation to generate addition products, and the characteristic peaks of addition product ions are observed in the mass spectrum of the reaction results, realizing the qualitative detection of these 10 kinds of sma...

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Abstract

The invention provides a phosphorus carpentine positive ion and a gas-phase preparation and application thereof. The method adopts a mass spectrometry device for gas-phase molecular-ion reaction and includes: dissolving triphenyl methyl bromide in methyl alcohol, wherein a mass spectrometry signal m / z 277 of triphenyl methyl phosphorus positive ion can be detected in an electrospray ionization-mass spectrometry positive ion mode; subjecting a mass spectra peak of m / z 277 to secondary mass spectra fragmentation through collision induced dissociation (CID) to obtain peak fragments m / z 185, namely the diphenyl phosphorous carpentine ion. The method is simple and easy to implement, small organic molecules are detected through reaction of the diphenyl phosphorous carpentine ion and the small organic molecules, the molecular-ion reaction is applied to detection of the trace organic molecules in the air, rapid qualitative and quantitative testing of the small organic molecules can be realized, some isomers can be distinguished according to difference of reaction results, and high flexibility is achieved.

Description

technical field [0001] The invention relates to the technical field of mass spectrum fragmentation and gas phase reaction, in particular to a phosphorus carbene cation and its gas phase preparation method and its application in the qualitative detection of small organic molecules. Background technique [0002] Mass spectrometer is a scientific analytical instrument with fast analysis speed, high sensitivity and molecular specificity. It is widely used in many fields such as chemistry, biology, environmental monitoring, medical and health. As a homogeneous reaction in mass spectrometry, gas phase reaction includes unimolecular reaction, bimolecular reaction and multimolecular reaction. Since the cluster effect and the influence on ions and solvent molecules are excluded in the gas phase, it has great potential in the study of reaction mechanism. unique advantage. Most ion reactions in mass spectrometry are unimolecular reactions, including isomerization and fragmentation of ...

Claims

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Application Information

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IPC IPC(8): C07F9/50G01N27/62
Inventor 潘远江尹欣驰方向熊行创
Owner ZHEJIANG UNIV
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