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Salt-tolerant liquid chromatography, electrospray mass spectrometry coupled interface device and method of using the same

A technology of electrospray mass spectrometry and liquid chromatography, applied in the field of liquid chromatography-mass spectrometry, to achieve the effects of enhanced detection sensitivity, less sample consumption, and rapid sample detection

Active Publication Date: 2017-05-24
CHENGDU INST OF BIOLOGY CHINESE ACAD OF S
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the flow rate used in general HPLC is 0.8-1mL / min, even for ultra-high performance liquid chromatography, the commonly used flow rate is 0.2-0.4mL / min, which is far greater than the sampling capacity of PESI (the sampling volume is generally Therefore, at present, PESI technology is only found in the field of direct analysis mass spectrometry, and its connection with the liquid phase channel to realize liquid phase mass spectrometry has not been reported yet.

Method used

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  • Salt-tolerant liquid chromatography, electrospray mass spectrometry coupled interface device and method of using the same
  • Salt-tolerant liquid chromatography, electrospray mass spectrometry coupled interface device and method of using the same
  • Salt-tolerant liquid chromatography, electrospray mass spectrometry coupled interface device and method of using the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 as figure 1 and figure 2 As shown, a salt-resistant liquid chromatography electrospray mass spectrometry interface device mainly includes: liquid phase spray generation module 1, rotating block module 2, probe high-voltage on-off module 3 and power module 4;

[0038]Wherein, the liquid phase spray generating module includes a liquid nozzle 11, an air nozzle 12, an air pipeline 13 and a liquid pipeline 14; one end of the liquid nozzle is connected to the liquid pipeline, and the liquid pipeline is connected to the liquid chromatography. Connected; one end of the gas path nozzle is connected to the gas path pipeline, and the gas path channel is connected to the atomized gas; the outlet end of the liquid path nozzle protrudes 1 mm laterally from the outlet end of the gas path nozzle;

[0039] The rotating block module includes an insulating part 21 and a block 22; the block is composed of two sets of block leaves 221 and block gaps 222, and the fan angle of the...

Embodiment 2

[0050] The similarities with Embodiment 1 will not be repeated, the difference is that: the outlet end of the liquid path nozzle is 0.5mm protruding from the outlet end of the gas path nozzle, and the flap has a fan-shaped flap gap with an angle of 120 degrees , the position of the insulating part of the conductive half-ring component corresponds to the notch of the blocking plate; the maximum speed of the electric motor is 1500rpm.

Embodiment 3

[0052] In order to test the effect of the present invention, the device provided in Example 1 and Waters I Class UPLC / Xevo TQ MS (Waters Group, USA) were used to carry out comparative experimental research on high-salt reserpine (1% NaCl).

[0053] 1. Experimental materials

[0054] 1.1 Analytes to be measured

[0055] Reserpine standard product (National Institute for Food and Drug Control, Beijing), batch number: 100041-201213. First use 1% formic acid methanol to make a 1mg / mL mother solution, and store it properly in the refrigerator. During the experiment, dilute it with methanol to a suitable concentration for the experiment.

[0056] 1.2 1% sodium chloride methanol solution (A)

[0057] Weigh 5g of sodium chloride (analytical grade, Chengdu Kelong Chemical Reagent Factory), add 100mL of high-purity water to dissolve, then add 400mL of methanol, and ultrasonically mix for 30min.

[0058] 2 Experimental methods

[0059] Column: ACQUITY UPLC BEH-C 18 Column, the packi...

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Abstract

The invention provides an anti-salt liquid chromatogram and electro-mist mass spectrometry combined interface device. The device mainly comprises a liquid phase mist generation module, a rotary barrier piece module, a probe high-voltage make-and-break module and a power module, the rotary barrier piece module comprises an insulating part and a barrier piece, one end of the insulating part is fixedly connected with the barrier piece, and the barrier piece is composed of barrier blades and barrier piece notches; one end of the probe high-voltage make-and-break module is connected with high voltage, and the other end of the probe high-voltage make-and-break module is connected with a conducting probe. According to the anti-salt liquid chromatogram electro-spray mass spectrometry combined interface device, by selecting the barrier piece notches of different sector angles or adjusting the rotation speed of the power module, the sampling capacity (the sampling quantity is generally several nano-liters) of the PESI conducting probe is satisfied, and combination of the liquid phase and the mass spectrum (PESI) is achieved. Meanwhile, the sharp end of the conducting probe generates electro-mist, so that unionized salt is deposited on the surface of the conducting probe, the problem that a high-salt sample access is blocked due to salt deposition is avoided, the detection sensitivity of the mass spectrum for a target compound in a high-salt base material is enhanced, and the liquid chromatogram and mass spectrometry coupling technology of a high-salt sample is achieved.

Description

technical field [0001] The invention relates to a salt-tolerant liquid chromatography-mass spectrometry interface device and a use method thereof, belonging to the technical field of liquid chromatography-mass spectrometry. Background technique [0002] Liquid chromatography-mass spectrometry (LC-MS) is also called liquid chromatography-mass spectrometry technology. Liquid chromatography-mass spectrometry is mainly composed of liquid chromatography, interface device (also an ion source), mass spectrometry and data processing system. Liquid chromatography is used as the separation system, and mass spectrometry is used as the detection system. The sample is separated from the mobile phase in the mass spectrometer, and after being ionized, the ion fragments are separated by the mass analyzer by the mass spectrometer, and the mass spectrogram is obtained by the detector. Liquid chromatography-mass spectrometry embodies the complementary advantages of chromatography and mass spe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 夏兵周燕马风伟季宝成丁立生
Owner CHENGDU INST OF BIOLOGY CHINESE ACAD OF S
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