An electrospray detector

By employing a straight-cylinder drift tube and migration tube, an electric field device, a heat insulation layer, and a charge neutralization device, the problems of sample loss and contamination in electrospray detectors have been solved, achieving high-precision and high-efficiency detection results.

CN116037339BActive Publication Date: 2025-12-23SUZHOU QUANPU INSTR TECH CO LTD
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202310069569.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-02-07
Publication Date
2025-12-23
Estimated Expiration
2043-02-07

AI Technical Summary

Technical Problem

Existing electrospray detectors suffer from sample loss and pipe contamination due to their curved tube structure, resulting in low detection accuracy and high detection costs.

Method used

A straight-cylinder drift tube and migration tube are used, combined with high-pressure gas atomization and electric field devices to avoid sample collision and condensation. An insulation layer and charge neutralization device are set up to control the gas flow rate.

Benefits of technology

It improves detection accuracy, reduces sample loss and tube wall contamination, ensures sample integrity and detection efficiency, and reduces detection costs.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN116037339B_ABST
    Figure CN116037339B_ABST
Patent Text Reader

Abstract

The application discloses an electrospray detector, which comprises a first air inlet pipe, a second air inlet pipe, a discharge chamber, an atomization chamber, a drift tube, a mixing chamber, a waste liquid pipe, a waste liquid bottle, a migration pipe, a particle removal trap and a collection device. The air inlet of the second air inlet pipe is communicated with the pipe body of the first air inlet pipe; the discharge chamber is communicated with the second air inlet pipe; the atomization chamber is communicated with the first air inlet pipe; the drift tube is formed in a straight cylinder shape; the drift tube is communicated with the atomization chamber; the mixing chamber is communicated with the drift tube and the discharge chamber; the waste liquid pipe is communicated with the mixing chamber; the liquid outlet of the waste liquid pipe is communicated with the waste liquid bottle; the migration pipe is communicated with the mixing chamber; the migration pipe is formed in a straight cylinder shape; the migration pipe and the drift tube are located on the same axis; the particle removal trap is arranged in the migration pipe; and the collection device is communicated with the migration pipe. The drift tube and the migration pipe of the electrospray detector are both in a straight cylinder shape, so that the sample does not collide with the pipe wall, the loss of the sample is avoided, the detection precision is improved, and the pollution to the pipe wall is reduced.
Need to check novelty before this filing date? Find Prior Art

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of drug detection, and particularly relates to an electrospray detector. BACKGROUND

[0002] The detection technology of the proportion of drug components is based on the characteristics of the chemical structure, polarity, molecular weight size or optical properties of the compounds contained in the drug. At present, corresponding detection technologies have been developed on the market for various characteristics, but the detection of drug components needs to detect multiple compounds in the drug, and the response values of different compounds to the detection technology for a certain characteristic are different. For example, a drug contains A compound and B compound, and the detection technology based on the chemical structure characteristics has a high response value for A compound and a low response value for B compound, and the detection technology for the polarity characteristics has a high response value for B compound. If only the detection technology based on the chemical structure characteristics is used, the B compound cannot be accurately detected, and if two detection technologies are used to detect A and B respectively, although the detection accuracy can be ensured, the detection cost is also increased.

[0003] Therefore, researchers have designed an electrospray detector, which can detect all non-volatile substances and is not affected by the characteristics of the compounds, and the response to various compounds is basically consistent. The specific detection process is as follows: before detection, each compound of the drug is eluted by an elution device, wherein elution refers to the process of separating different components in the sample by selecting a suitable solvent for flow washing during chromatographic separation; after obtaining the eluent of each compound, the eluent containing a certain compound is introduced into the atomization chamber of the electrospray detector, and the drug eluent is atomized by nitrogen, wherein the large droplets that are not completely atomized flow out through the shunt structure, and the small droplets that are completely atomized enter the drift tube; the solvent in the atomized small droplets is evaporated and dried in the drift tube to obtain solute particles; the solute particles enter the mixing chamber and collide with the charged nitrogen to carry electric charges; finally, the electric charges are collected by a charge collection device and converted into an electric signal to be transmitted to the matching software for analysis and processing.

[0004] However, the current electrospray detector has many curved pipe structures and shunt structures, which are not convenient to clean and maintain, and the atomized droplets flowing through the curved pipe structure will collide with the pipe wall, causing sample loss and pipe contamination. In addition, the large droplets are also excluded through the shunt structure, which also causes sample loss and reduces the detection accuracy. SUMMARY

[0005] The electric spray detector provided by the application overcomes the defects of the prior art, the drift tube and the migration tube are both straight cylinders, the central axes of the drift tube and the migration tube are in a straight line, the sample does not need to pass through a curved structure and collide with the tube wall in the process of reaching the collection device from the atomization chamber, loss of the sample is avoided, detection accuracy is improved, and pollution to the tube wall is greatly reduced.In addition, the electric spray detector repeatedly atomizes the eluent in the atomization chamber by using high-pressure gas, so that the atomization of the eluent is more thorough, the appearance of large droplets is avoided, the shunt structure is omitted, the integrity of the sample is ensured, and the detection accuracy is improved.

[0006] To achieve the above object, the technical scheme adopted by the application is:

[0007] The electric spray detector provided by the application comprises:

[0008] A first gas inlet pipe, an air inlet of the first gas inlet pipe is used for receiving high-pressure gas;

[0009] A second gas inlet pipe, an air inlet of the second gas inlet pipe is communicated with a pipe body of the first gas inlet pipe;

[0010] A discharge chamber, the discharge chamber is provided with an air inlet and an air outlet, the air inlet of the discharge chamber is communicated with the air outlet of the second gas inlet pipe, and an electrode probe is arranged in the discharge chamber and used for loading charges on the high-pressure gas;

[0011] An atomization chamber, the atomization chamber is provided with a sample inlet, a gas inlet and a sample outlet, the sample inlet of the atomization chamber is used for receiving sample eluent, and the gas inlet of the atomization chamber is communicated with the air outlet of the first gas inlet pipe;

[0012] A drift tube, the drift tube is formed in a straight cylinder, a sample inlet of the drift tube is communicated with the sample outlet of the atomization chamber, and a temperature control heating device is arranged on the drift tube and used for evaporating solvents in the atomized sample eluent into a gaseous state;

[0013] A mixing chamber, the mixing chamber is provided with a sample inlet, a sample outlet, a gas inlet and a gas outlet, the sample inlet of the mixing chamber is communicated with the sample outlet of the drift tube, and the gas inlet of the mixing chamber is communicated with the gas outlet of the discharge chamber;

[0014] A waste liquid pipe and a waste liquid bottle, a liquid inlet of the waste liquid pipe is communicated with the gas outlet of the mixing chamber, and a liquid outlet of the waste liquid pipe is communicated with the waste liquid bottle;

[0015] A migration tube and a particle removal trap, the migration tube is formed in a straight cylinder, a sample inlet of the migration tube is communicated with the sample outlet of the mixing chamber, the migration tube and the drift tube are located on the same axis, and the particle removal trap is arranged in the migration tube and used for separating charges in the charged particles;

[0016] A collection device is connected to the sample outlet of the transfer tube for collecting the separated electric charges and delivering them to a charge meter.

[0017] In a preferred embodiment of the present application, an electric field device is arranged on the transfer tube for applying an electric field to the charged particles to increase their kinetic energy.

[0018] In a preferred embodiment of the present application, the electrospray detector further comprises a heat insulation layer covering the outside of the drift tube, the mixing chamber and the transfer tube.

[0019] In a preferred embodiment of the present application, a charge neutralization device is arranged in the waste liquid pipe for neutralizing the electric charges flowing through the waste liquid pipe.

[0020] In a preferred embodiment of the present application, the gas inlet of the mixing chamber and the gas outlet of the mixing chamber are respectively arranged on the upper and lower sides of the mixing chamber, and the sample inlet of the mixing chamber and the sample outlet of the mixing chamber are respectively arranged on the left and right sides of the mixing chamber.

[0021] In a preferred embodiment of the present application, the electrospray detector further comprises a gas path valve arranged at the gas inlet end of the first gas inlet tube.

[0022] In a preferred embodiment of the present application, the electrospray detector further comprises a gas flow controller arranged at the connection between the first gas inlet tube and the second gas inlet tube for controlling the gas flow into both.

[0023] In a preferred embodiment of the present application, the electrode probe is a high-voltage platinum electrode probe.

[0024] The present application solves the defects in the background art and has at least the following beneficial effects:

[0025] (1) The drift tube and the transfer tube of the electrospray detector of the present application are both straight cylinders, and the central axes of the drift tube and the transfer tube are in a straight line. The sample does not need to pass through a curved structure from the atomization chamber to the collection device, and will not collide with the tube wall, avoiding the loss of the sample, improving the detection accuracy, and greatly reducing the pollution to the tube wall. In addition, the electrospray detector of the present application repeatedly atomizes the eluent in the atomization chamber by high-pressure gas, making the atomization of the eluent more thorough, avoiding the appearance of large droplets, thereby eliminating the need for a flow splitting structure, ensuring the integrity of the sample, and improving the detection accuracy.

[0026] (2) The eluent mainly relies on its own inertia to move from the atomization chamber to the collection device. When the atomized eluent reaches the mixing chamber, the kinetic energy has been greatly reduced, and the subsequent movement is relatively slow. The electric field device is arranged on the migration tube, an electric field is applied in the migration tube by the electric field device, the kinetic energy of the charged particles is increased, and the movement of the charged particles is accelerated, so that the detection efficiency is improved.

[0027] (3) If the temperature decreases after the solvent in the atomized eluent evaporates into a gas, the solvent may condense into droplets. After the droplets combine with solute particles, the degree of combination with electric charges increases, resulting in an increase in combined electric charges, thereby affecting the detection accuracy. The entire flow channel of the eluent is covered by the heat preservation layer, so that the temperature is constant, the gaseous solvent is prevented from condensing, and the detection accuracy is ensured.

[0028] (4) The electric charge neutralization device is arranged in the waste liquid pipe to neutralize the electric charges in the waste liquid, so that the safety hazard of the waste liquid is eliminated.

[0029] (5) The gas flow controller of the electric spray detector is arranged at the connection between the first gas inlet pipe and the second gas inlet pipe. The gas flow controller controls the gas flow entering the two pipes respectively, so that different gas flows can be used for different eluents, and the atomization and collision effects are always optimal. BRIEF DESCRIPTION OF DRAWINGS

[0030] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed in the following embodiment or prior art description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor;

[0031] Figure 1 is a perspective view of the electric spray detector of the preferred embodiment of the present application;

[0032] Figure 2 is a cross-sectional view of the electric spray detector of the preferred embodiment of the present application;

[0033] The drawings are as follows: 1. First gas inlet pipe; 2. Second gas inlet pipe; 3. Discharge chamber; 4. Atomization chamber; 5. Drift tube; 6. Mixing chamber; 7. Waste liquid pipe; 8. Waste liquid bottle; 9. Migration tube; 10. Particle removal trap; 11. Collection device; 12. Electrode probe; 13. Heat preservation layer; 14. Electric charge neutralization device; 15. Gas path valve; 16. Gas flow controller. DETAILED DESCRIPTION

[0034] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0035] Many specific details are set forth in the following description in order to provide a full understanding of the invention. However, the invention may also be practiced in other ways different from those described herein. Therefore, the scope of protection of the invention is not limited to the specific embodiments disclosed below.

[0036] In the description of this application, it should be understood that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicating orientation or positional relationships based on the orientation or positional relationships shown in the accompanying drawings, are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as limiting the scope of protection of this application. Furthermore, the terms "first," "second," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Therefore, features defined with "first," "second," etc., may explicitly or implicitly include one or more of that feature. In the description of this invention, unless otherwise stated, "a plurality of" means two or more.

[0037] In the description of this application, it should be noted that, unless otherwise expressly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to mechanical connections or electrical connections; they can refer to direct connections or indirect connections through an intermediate medium; and they can refer to the internal communication between two components. Those skilled in the art will understand the specific meaning of the above terms in this application based on the specific circumstances.

[0038] Example 1

[0039] like Figure 1 , Figure 2As shown, the electrospray detector of the embodiment comprises a first gas inlet pipe 1, a second gas inlet pipe 2, a discharge chamber 3, an atomization chamber 4, a drift tube 5, a mixing chamber 6, a waste liquid pipe 7, a waste liquid bottle 8, a migration tube 9, a particle removal trap 10 and a collection device 11. The discharge chamber 3 is provided with an electrode probe 12. The drift tube 5 is provided with a temperature control heating device (not shown in the figure). The first gas inlet pipe 1 is used to receive high-pressure gas. The gas inlet of the second gas inlet pipe 2 is connected to the pipe body of the first gas inlet pipe 1. The discharge chamber 3 is provided with a gas inlet and a gas outlet. The gas inlet of the discharge chamber 3 is connected to the gas outlet of the second gas inlet pipe 2. The electrode probe 12 in the discharge chamber 3 is used to charge the high-pressure gas. The atomization chamber 4 is provided with a sample inlet, a gas inlet and a sample outlet. The sample inlet of the atomization chamber 4 is used to receive sample eluent. The gas inlet of the atomization chamber 4 is connected to the gas outlet of the first gas inlet pipe 1. The drift tube 5 is in a straight cylindrical shape. The sample inlet of the drift tube 5 is connected to the sample outlet of the atomization chamber 4. The drift tube 5 is provided with a temperature control heating device, which is used to evaporate the solvent in the atomized sample eluent into a gaseous state. The mixing chamber 6 is provided with a sample inlet, a sample outlet, a gas inlet and a gas outlet. The sample inlet of the mixing chamber 6 is connected to the sample outlet of the drift tube 5. The gas inlet of the mixing chamber 6 is connected to the gas outlet of the discharge chamber 3. The liquid inlet of the waste liquid pipe 7 is connected to the gas outlet of the mixing chamber 6. The liquid outlet of the waste liquid pipe 7 is connected to the waste liquid bottle 8. The migration tube 9 is in a straight cylindrical shape. The sample inlet of the migration tube 9 is connected to the sample outlet of the mixing chamber 6. The migration tube 9 and the drift tube 5 are located on the same axis. The particle removal trap 10 is arranged in the migration tube 9 and is used to separate the electric charge in the charged particles. The collection device 11 is connected to the sample outlet of the migration tube 9 and is used to collect the separated electric charge and deliver it to a charge meter.

[0040] The operation principle of the electrospray detector of the embodiment is as follows: first, elute each compound contained in the medicine to be detected by the elution device; then, high-pressure gas is introduced into the gas inlet of the first gas inlet pipe 1, and the high-pressure gas is selected from inert gas, and nitrogen can be selected in the embodiment; after the gas enters the first gas inlet pipe 1, it is divided into two gas streams, one gas stream blows along the first gas inlet pipe 1 to the atomization chamber 4, and the other gas stream blows along the second gas inlet pipe 2 to the discharge chamber 3; the electrode probe 12 in the discharge chamber 3 is opened, and the electrode probe 12 discharges to make the gas flowing through the electrode probe 12 carry electric charge, and the gas carrying electric charge blows into the mixing chamber 6; then, the eluent of a certain compound is continuously injected from the sample inlet of the atomization chamber 4, and the high-pressure gas blown by the first gas inlet pipe 1 repeatedly atomizes the injected eluent to ensure that the eluent is completely atomized; the atomized eluent enters the drift tube 5, and the temperature control heating device in the drift tube 5 heats the atomized eluent, so that the solvent in the atomized eluent is evaporated into gas, thereby obtaining solute particles; the solute particles drift to the mixing chamber 6 and collide with the gas carrying electric charge blown from the discharge chamber 3, and the solute particles obtain electric charge from the gas after the collision; the gas blown from the discharge chamber 3 also blows the gaseous solvent and free electric charge in the mixing chamber 6 to the waste liquid pipe 7, and the gaseous solvent and free electric charge are condensed into droplets after passing through the waste liquid pipe 7 and finally flow into the waste liquid bottle 8; the solute particles carrying electric charge drift to the migration tube 9 and collide with the particle removal trap 10 in the migration tube 9, and the solute particles are blocked after the collision, and the electric charge on the solute particles is filtered out and flows to the collection device 11; finally, the electric charge is collected by the electric charge collection device 11 and converted into an electric signal by the electric charge meter for transmission to the matching software for analysis and processing.

[0041] Since the electric signal is proportional to the number of electric charges carried by the solute particles, the number of electric charges carried by the solute particles is proportional to the area of the solute particles, and the area of the solute particles is proportional to the mass of the solute particles, therefore, the ratio of the electric signals corresponding to various compounds can be detected, and the mass ratio between each compound can be detected.

[0042] The drift tube 5 and the migration tube 9 of the electrospray detector of the embodiment are both straight cylinders, and the central axes of the drift tube 5 and the migration tube 9 are on the same straight line, so that the sample does not need to pass through a curved structure from the atomization chamber 4 to the collection device 11 and does not collide with the tube wall, thereby avoiding the loss of the sample, improving the detection accuracy, and greatly reducing the pollution of the tube wall. In addition, the electrospray detector of the embodiment repeatedly atomizes the eluent in the atomization chamber 4 by high-pressure gas, so that the eluent is completely atomized and the appearance of large droplets is avoided, thereby eliminating the shunt structure, ensuring the integrity of the sample, and improving the detection accuracy.

[0043] In this embodiment, the migration tube 9 is provided with an electric field device for applying an electric field to the charged particles to increase their kinetic energy. The eluent mainly relies on its own inertia to advance from the atomization chamber 4 to the collection device 11. When the atomized eluent reaches the mixing chamber 6, the kinetic energy has been greatly reduced, and the subsequent movement is relatively slow. Therefore, by applying an electric field in the migration tube 9 through the electric field device, the kinetic energy of the charged particles is increased, the movement of the charged particles is accelerated, and the detection efficiency is improved.

[0044] In this embodiment, a heat preservation layer 13 is also included, which covers the outside of the drift tube 5, the mixing chamber 6, and the migration tube 9. After the solvent in the atomized eluent evaporates into gas, if the temperature decreases, the gaseous solvent may condense into droplets, which, after combining with the solute particles, will increase the degree of combination with the electric charge, resulting in an increase in the combined electric charge, thereby affecting the detection accuracy. By covering the entire flow path of the eluent with the heat preservation layer 13, the temperature is stabilized, preventing the condensation of gaseous solvent, and ensuring the detection accuracy.

[0045] In this embodiment, the waste liquid pipe 7 is provided with a charge neutralization device 14 for neutralizing the electric charge flowing through the waste liquid pipe 7. If the charged waste liquid from the mixing chamber 6 is not subjected to charge removal treatment, there may be a safety hazard. In this embodiment, the charge neutralization device 14 neutralizes the electric charge in the waste liquid, eliminating the safety hazard of the waste liquid.

[0046] In this embodiment, the gas inlet of the mixing chamber 6 and the gas outlet of the mixing chamber 6 are located on the upper and lower sides of the mixing chamber 6, respectively, and the sample inlet of the mixing chamber 6 and the sample outlet of the mixing chamber 6 are located on the left and right sides of the mixing chamber 6, respectively. The gas channels formed by the gas inlet and the gas outlet of the mixing chamber 6 and the gas channels formed by the sample inlet and the sample outlet of the mixing chamber 6 are cross-shaped, which not only ensures sufficient collision between the charged gas and the atomized eluent, but also ensures the rationality of the structure, facilitating disassembly and cleaning.

[0047] In this embodiment, a gas path valve 15 is also included, which is arranged at the gas inlet end of the first gas inlet pipe 1.

[0048] In this embodiment, a gas flow controller 16 is also included, which is arranged at the connection between the first gas inlet pipe 1 and the second gas inlet pipe 2, for controlling the gas flow into the two pipes. In this embodiment, the gas flow controller 16 controls the gas flow into the two pipes separately, allowing different gas flows for different eluents to ensure that the atomization and collision effects are always optimal.

[0049] In this embodiment, the electrode probe 12 is a high-voltage platinum electrode probe.

[0050] The above is based on the ideal embodiment of the application, through the above description, relevant personnel can make various changes and modifications without deviating from the technical idea of the application. The technical scope of the application is not limited to the content of the specification, and the technical scope must be determined according to the scope of claims.

Claims

1. An electrospray detector characterized by, It comprises: a first gas inlet pipe, the gas inlet of which is used for receiving high-pressure gas; a second gas inlet pipe, the gas inlet of which is communicated with the pipe body of the first gas inlet pipe; a discharge chamber, which is provided with a gas inlet and a gas outlet, the gas inlet of the discharge chamber is communicated with the gas outlet of the second gas inlet pipe, and an electrode probe is arranged in the discharge chamber for charging the high-pressure gas; an atomization chamber, which is provided with a sample inlet, a gas inlet and a sample outlet, the sample inlet of the atomization chamber is used for receiving sample eluent, and the gas inlet of the atomization chamber is communicated with the gas outlet of the first gas inlet pipe; a drift tube, which is formed in a straight cylinder shape, the sample inlet of the drift tube is communicated with the sample outlet of the atomization chamber, and a temperature control heating device is arranged on the drift tube for evaporating the solvent in the atomized sample eluent into a gaseous state; a mixing chamber, which is provided with a sample inlet, a sample outlet, a gas inlet and a gas outlet, the sample inlet of the mixing chamber is communicated with the sample outlet of the drift tube, and the gas inlet of the mixing chamber is communicated with the gas outlet of the discharge chamber; wherein the gas inlet and the gas outlet of the mixing chamber are respectively located on the upper and lower sides of the mixing chamber, and the sample inlet and the sample outlet of the mixing chamber are respectively located on the left and right sides of the mixing chamber, forming a cross-shaped gas flow channel; a waste liquid pipe and a waste liquid bottle, the liquid inlet of the waste liquid pipe is communicated with the gas outlet of the mixing chamber, and the liquid outlet of the waste liquid pipe is communicated with the waste liquid bottle; a migration tube and a particle removal trap, the migration tube is formed in a straight cylinder shape, the sample inlet of the migration tube is communicated with the sample outlet of the mixing chamber, the migration tube is located on the same axis as the drift tube, and the particle removal trap is arranged in the migration tube for separating the electric charge from the charged particles; an electric field device is arranged on the migration tube for applying an electric field to the charged particles to increase their kinetic energy; a collection device, which is communicated with the sample outlet of the migration tube, is used for collecting the separated electric charge and conveying it to an electric charge meter; a gas flow controller, which is arranged at the connection between the first gas inlet pipe and the second gas inlet pipe, is used for controlling the gas flow into the two pipes.

2. An electrospray detector according to claim 1, wherein, It further comprises a heat preservation layer, which covers the outer sides of the drift tube, the mixing chamber and the migration tube.

3. An electrospray detector according to claim 1, wherein, The waste liquid pipe is provided with a charge neutralization device, which is used for neutralizing the electric charge flowing through the waste liquid pipe.

4. An electrospray detector according to claim 1, wherein, It further comprises a gas path valve, which is arranged at the gas inlet end of the first gas inlet pipe.

5. An electrospray detector according to claim 1, wherein, The electrode probe adopts a high-voltage platinum electric needle.

Citation Information

Patent Citations

  • Analyzing device and analyzing method for trace impurities in organic pure substance

    CN103149283A

  • Corona discharge atomization particle live-line detector

    CN104181263A