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Liquid chromatography-mass spectrometry detection method capable of directly analyzing salt-containing sample based on electric arc thermal coupling

A technology of liquid chromatography-mass spectrometry and detection method, applied in the field of liquid chromatography-mass spectrometry, can solve problems such as single arc quenching, and achieve the effects of rapid sample detection, enhanced detection sensitivity, and simple instrument construction

Pending Publication Date: 2021-11-30
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the flow rate used in general high-performance liquid chromatography is 0.8-1.5mL / min. Even for ultra-high-performance liquid chromatography, the commonly used working flow rate is 0.2-0.8mL / min. A single arc causes the quenching of a single arc

Method used

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  • Liquid chromatography-mass spectrometry detection method capable of directly analyzing salt-containing sample based on electric arc thermal coupling
  • Liquid chromatography-mass spectrometry detection method capable of directly analyzing salt-containing sample based on electric arc thermal coupling
  • Liquid chromatography-mass spectrometry detection method capable of directly analyzing salt-containing sample based on electric arc thermal coupling

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] In order to test the effect of the present invention, the device provided in Experimental Operation 1 and the ultimate UPLC / LTQ Orbitrap mass spectrometer (Thermo Fisher Corporation of the United States) were used to carry out comparative experimental research on high-salt DHT.

[0086] 1. Experimental materials

[0087] 1.1 Analytes to be measured

[0088] DHT standard substance (analytical grade, Hangzhou Chentong Materials Co., Ltd.), batch number: M832366. First make a 1mg / mL mother solution with methanol, store it properly in the refrigerator, and dilute it with methanol to an appropriate concentration for the experiment.

[0089] 1.2 Methanol salt solution

[0090] Weigh 5 g of sodium chloride (analytical grade, Hangzhou Ron Chemical Co., Ltd.), add 100 mL of high-purity water to dissolve, then add 400 mL of methanol, and ultrasonically mix for 30 min to finally obtain a 1% methanol solution of sodium chloride.

[0091] Weigh 5 g of lithium chloride (analytical...

Embodiment 2

[0108] In order to further test the effect of the present invention, the device provided in Experimental Operation 1 and the ultimate UPLC / LTQ Orbitrap mass spectrometer (Thermo Fisher Corporation of the United States) were used to carry out experimental research on Rhodamine B (Rhodamine) in the buffer salt system.

[0109] 1. Experimental materials

[0110] 1.1 Analytes to be measured

[0111] Rhodamine B standard product (analytical grade, Hangzhou Bangyi Chemical Co., Ltd.), batch number: R006869. First make a 1mmol / L mother liquor with methanol, store it properly in the refrigerator, and dilute it with methanol to a suitable concentration for the experiment.

[0112] 1.2 Buffered saline solution

[0113] Measure 10 mL of PBS buffer solution (analytical grade, Hangzhou Bangyi Chemical Co., Ltd.) with a pH of 7 and a concentration of 1 mol / L, add 90 mL of high-purity water to dissolve, and mix by ultrasonic for 30 minutes to prepare a 100 mmol / L PBS buffer solution.

[0...

Embodiment 4

[0129] In order to further test the effect of the present invention, the device provided in Experimental Operation 1 and the ultimate UPLC / LTQ Orbitrap mass spectrometer (Thermo Fisher Corporation, USA) were used to carry out experimental research on reserpine in the buffer salt system.

[0130] 1. Experimental materials

[0131] 1.1 Analytes to be measured

[0132] Reserpine standard product (analytical grade, Hangzhou Bangyi Chemical Co., Ltd.), batch number: R006853. First make a 1mmol / L mother solution with acetone, store it properly in the refrigerator, and dilute it with acetone to a suitable concentration for the experiment.

[0133] 1.2 Buffered saline solution

[0134] The preparation method of the buffered saline solution is the same as that in Example 2.

[0135] 2 Experimental methods

[0136] Aspirate 0.5mL of 1mmol / L reserpine and add it into 4.5mL of acetone to make a 100μmol / L standard solution.

[0137] Draw 500 μL of reserpine standard solution and 500 μ...

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Abstract

The invention discloses a liquid chromatography-mass spectrometry detection method capable of directly analyzing a salt-containing sample based on electric arc thermal coupling, which comprises the following steps that 1) sample atomization is conducted, the spraying direction of a liquid phase spraying generation module is adjusted, the direction pointed by a nozzle is the tip of a metal heat source with a tip, after being separated by liquid chromatography, the sample enters a liquid path pipeline of the liquid phase spray generation module and flows out from a liquid path spray head, atomized gas is sprayed out from a gas path spray head 112 through a gas path pipeline, and the sample in the liquid path spray head is atomized into small liquid drops under the action of the atomized gas; and 2) ionization is conducted, the atomized droplets are sprayed on a metal heat source which is coupled with the electric arc and is provided with a tip, the metal heat source with the tip ionizes the droplets to generate gas phase ions, and then the gas phase ions enter mass spectrometry to realize efficient ionization analysis of the charged ions. The liquid chromatography combination is achieved, and the efficient separation characteristic of the liquid chromatography and the high salt tolerance characteristic of the AEAI are fused;.

Description

technical field [0001] The invention relates to the technical field of liquid chromatography-mass spectrometry, in particular to a liquid chromatography-mass spectrometry detection method based on arc thermal coupling that can directly analyze salt-containing samples. Background technique [0002] Liquid chromatography-mass spectrometry (LC-MS), also known as liquid chromatography-mass spectrometry, is mainly composed of liquid chromatography, an interface device (also an ion source), mass spectrometry, and a data processing system. The principle is to use the excellent separation ability of liquid chromatography as a separation system to separate samples according to their polarity, and then use high-sensitivity mass spectrometry to detect different samples. The sample after liquid phase separation is ionized by the ion source, and then separated according to the mass-to-charge ratio in the mass analyzer of the mass spectrometer, and finally the mass spectrum is obtained th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/726
Inventor 潘远江高元吉陈维伟
Owner ZHEJIANG UNIV
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