Mass spectra ion source without external high pressure and ionization analytical method thereof

An analysis method and ion source technology, applied in the field of food safety testing, can solve problems such as restrictions, electrospray capillary prone to corona discharge, and complicated instrument design

Inactive Publication Date: 2008-01-30
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the traditional DESI ion source requires an external high-voltage power supply to build a high-voltage electrostatic field between the zero-potential mass spectrometer sampling cone, the instrument design is complicated.
More importantly, due to the existence of an external hi...

Method used

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  • Mass spectra ion source without external high pressure and ionization analytical method thereof
  • Mass spectra ion source without external high pressure and ionization analytical method thereof
  • Mass spectra ion source without external high pressure and ionization analytical method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Use acetonitrile containing 0.1% formic acid: water=1:1 (v / v) as the spray solvent, the flow rate is 4μL / min, and the carrier gas (spray gas) is N 2 , The outlet pressure is 15psi, take 10μg / mL of 8 kinds of triazine herbicide mixture sample solution 2μL drop on the glass plate after hydrofluoric acid corrosion, the area is about 16mm 2 (Equivalent to 1250pg / mm 2 ), let the glass plate dry, then place it under the spray needle, apply a voltage of -4000v to the end of the mass spectrometer inlet capillary, and measure the temperature of the mass spectrometer's sampling port at 250°C to obtain a mass spectrum as shown in Figure 2. It can be seen from the figure that the compound can get very good [M+H] + Peak, which proves that this ionization source can identify the mixture well. The eight triazine herbicides are: Simatone [M+H] + m / z 198.33; Atrazine [M+H] + m / z216.35; Fighting through [M+H] + m / z 226.36; Ammiejing [M+H] + m / z 228.33; Cyanazine [M+H] + m / z241.31; PuMieJing[...

Embodiment 2

[0044] Use methanol containing 0.1% formic acid: water=1:1 (v / v) as spray solvent, flow rate 4μL / min, carrier gas as N 2 , The outlet pressure is 15 psi, apply terbucin (Mw 229) solution on a glass slide, then place the slide on the stage, aim at the spray needle, and apply a voltage of -450v to the end of the mass spectrometer inlet capillary. The temperature of the sampling port of the mass spectrometer is controlled at 250℃ for measurement. The MS and MS / MS spectra are shown in Figure 3. From the spectra, you can see obvious [M+H] + m / z 230 and [M+Na] + The m / z 252 peak and the cluster of isotopic peaks can be confirmed by MS / MS. It can be seen that at a certain concentration, the test compound can be ionized significantly [M+H] + And [M+Na] + peak.

Embodiment 3

[0046] Use acetonitrile containing 0.1% formic acid: water (1:1, v / v) as spray solvent, flow rate 4μL / min, carrier gas N 2 , The outlet pressure is 15psi, the mass spectrometer terminal voltage is -4500V, the sampling port temperature of the mass spectrometer is controlled at 250℃, and the glass plate corroded by hydrofluoric acid contains 625pg / mm 2 Of chlorpyrifos (Mw 349). The mass spectrum analysis chart is shown in Figure 4. The compound contains 3 chlorines. The isotope peak cluster response can be clearly seen in the mass spectrum m / z350:m / z352:m / z354:m / z356 =27:27:9:1, which proves that it is indeed the tested compound.

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Abstract

The invention discloses a mass spectra ion source without exterior high pressure and ionization analysis method, pertaining to food safety detective technology field. The ionization sources of the invention include electric atomizer, capillary, peristaltic pump, inert gas source and ionization source. The atomization system comprises the electric atomizer and the analyzed sample, the capillary is fixedly arranged at the center of the pipe of electric atomizer, an inlet duct is connected with the pipe of the electric atomizer in the lateral plane and connected with the inert gas source by stainless steel channel; the sampling outlet of the mass spectra is an ion collection analysis device while being arranged above the sample to be analyzed. The whole electric atomizer system does not adopt high pressure in any composition. When in use, person can directly hold the food by hand while rough scanning. The apparatus puts an end to the risk factor of high electric field exert by the electric atomizer, further the design of the apparatus is simple for disassembly, and the independent and standardized elements make the atomization system not prone to be polluted and can be applied in various food safety monitoring places.

Description

Technical field [0001] The invention belongs to the technical field of food safety detection, and particularly relates to a dedicated ion source and a mass spectrometry ion source without external high pressure that is directly safely ionized on a solid surface and an ionization analysis method thereof. Background technique [0002] In the field of food safety, especially the analysis of pesticide residues on various food surfaces is an important area related to the national economy and people's livelihood. At present, this field urgently needs a sensitive, fast, non-destructive, high-throughput analysis method that can directly obtain pesticide residue information from the sample surface without any pretreatment. This analytical method also requires that the analytical instrument must be simple in structure, easy to disassemble, difficult to contaminate, and can scan solid surfaces under various conditions of accuracy. [0003] The mass spectrometer is one of the most sensitive ...

Claims

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Application Information

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IPC IPC(8): G01N27/64H01J49/10G01N30/72
Inventor 赵孟夏张新忠张四纯韩昊马晓东李重九张新荣
Owner TSINGHUA UNIV
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