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Device and method for combining electrochemistry with electrospray ionization mass spectrometry

An electrospray ionization and electrochemical technology, applied in the field of analysis, can solve the problems of complex electrochemical reaction products, reduced electrochemical current efficiency, and inability to carry out quantitative analysis, so as to improve analysis efficiency and accuracy, reduce complexity, Avoid cross-talking effects

Inactive Publication Date: 2013-04-10
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the working electrode and the auxiliary electrode of the currently proposed electrochemical electrospray device are located in the flow path of the solution sample, no diaphragm is added between them to properly protect the product of the electrochemical reaction, so the electrochemical reaction occurs on the surface of the working electrode. The product of the product can easily diffuse to the surface of the auxiliary electrode and reverse the electrochemical reaction, and vice versa, which not only leads to a large decrease in the electrochemical current efficiency, but also in the process of multiple oxidation / reduction, coupled chemical Reactions such as radical polymerization and electrophilic or nucleophilic addition of solvents will also lead to complex electrochemical reaction products, reducing the accuracy of the analysis
Quantitative analysis will not be possible for most systems except for a few

Method used

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  • Device and method for combining electrochemistry with electrospray ionization mass spectrometry
  • Device and method for combining electrochemistry with electrospray ionization mass spectrometry
  • Device and method for combining electrochemistry with electrospray ionization mass spectrometry

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Embodiment 1

[0030] figure 2 and image 3 It is a structural schematic diagram of the first embodiment of the present invention. The solution sample is injected into the PEEK through a capillary 8 TM At the inlet end of the miniature tee, the outer diameter of the capillary is 1 / 16in, and the inner diameter is generally several hundred microns. Capillary tubes of other materials and sizes, such as fused silica capillary tubes, can also be used. The working electrode 1 is a platinum wire with a diameter of 0.5mm, and the leading end is covered with a sealing sleeve 7 and passed through the tee nut 9. The outer diameter of the sealing sleeve 7 is 1 / 16in, the inner diameter is 0.5mm, and the hole diameter of the nut is 1 / 16in, to match the outside diameter of the casing. The external thread of the nut matches the internal thread of the tee, and the material of the sleeve and the nut is PEEK TM , After being screwed into the tee, it plays a role of clamping and sealing. The electrochemi...

Embodiment 2

[0033] Figure 4 and Figure 5 It is a structural schematic diagram of the second embodiment of the present invention. The difference from the first embodiment is that the auxiliary electrode chamber 6 adds a sealing cover 14 to form a closed structure, and the auxiliary electrode chamber 6 increases an inlet 12 of the electrode liquid and an outlet 13 of the electrode liquid to facilitate the electrochemical reaction. Supplement or update the auxiliary electrode solution at any time during the process. Such a structure has wider adaptability, because the reactants that undergo electrochemical reactions on the surface of the auxiliary electrode are provided by the auxiliary electrode liquid itself, so the solution sample has a greater degree of freedom in selecting the supporting electrolyte. The cost is that during the working process, the auxiliary electrode liquid needs to be supplemented or renewed at any time to maintain the substances consumed on the auxiliary electrod...

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Abstract

The invention belongs to the technical field of analysis, in particular to a device and method for combining electrochemical and electrospray ionization mass spectrometry. The device of the invention consists of an electrochemical reactor and an electrospray ionization ion source. The electrochemical reactor includes a working electrode chamber and an auxiliary electrode chamber. The working electrode chamber and the auxiliary electrode chamber are separated by a diaphragm. The diaphragm has the function of preventing or delaying the exchange of neutral substances between the two electrode chambers and allowing ions or certain electric Sexual ion exchange. When the solution sample flows into the working electrode chamber, it is subjected to the electrochemical voltage loaded between the working electrode and the auxiliary electrode to undergo an electrochemical reaction. The product of the electrochemical reaction is protected by the diaphragm, and then forms gas-phase ions under the action of the electrospray ionization working voltage and enters the mass spectrometer for analysis. The invention also has the advantages of high electrochemical reaction efficiency, simple electrochemical reaction products, fast response speed, fastness, accuracy and high sensitivity suitable for quantitative analysis and mass spectrometry analysis.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to a device and a method for combining two analytical techniques of electrochemistry and electrospray ionization mass spectrometry. technical background [0002] Analytical techniques based on electrochemistry and electrospray ionization mass spectrometry are widely used in various fields such as scientific research, medical and health care, environmental monitoring and food safety. These two techniques are very complementary: electrochemistry has the advantages of fast, sensitive and quantitative, and can effectively distinguish species with large differences in electrical activity, but it does not have the ability to analyze structures. Mass spectrometry has strong structural analysis capabilities. Therefore, the combination of these two technologies can not only effectively improve the efficiency and accuracy of analysis, but also produce significant synergistic eff...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01J49/16G01N27/62
Inventor 凌星丁传凡
Owner FUDAN UNIV
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