CN110112051B - Vortex tube for mass spectrum reaction acceleration and signal enhancement and implementation method - Google Patents

Vortex tube for mass spectrum reaction acceleration and signal enhancement and implementation method Download PDF

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CN110112051B
CN110112051B CN201910419784.4A CN201910419784A CN110112051B CN 110112051 B CN110112051 B CN 110112051B CN 201910419784 A CN201910419784 A CN 201910419784A CN 110112051 B CN110112051 B CN 110112051B
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tube
mass spectrum
vortex tube
vortex
inlet
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CN110112051A (en
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聂宗秀
李玉泽
王光辉
熊彩侨
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Institute of Chemistry CAS
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components

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Abstract

The invention relates to a vortex tube for mass spectrum reaction acceleration and signal enhancement and an implementation method, belongs to the technical field of ion optical device manufacturing, and solves the problems of low ion transmission efficiency and ionization efficiency, low reactant ion mixing contact efficiency and difficult adjustment of reaction time in the reaction monitoring and reaction acceleration processes of mass spectra in the prior art. The vortex tube for the mass spectrum sample inlet comprises a sealing tube and a threaded tube with an axial ion channel, wherein the threaded tube is provided with an external thread and is arranged in the sealing tube, and a groove of the external thread is used as a gas channel; the vortex tube is arranged between the ion source and the mass spectrum sample inlet; the side wall of the sealing tube is provided with a gas flow inlet for introducing gas. The method for enhancing the mass spectrum signal comprises the steps of placing a vortex tube → injecting a sample → introducing nitrogen → entering mass spectrum detection. The invention realizes the enhancement of the response signal of the mass spectrum by arranging the vortex tube.

Description

Vortex tube for mass spectrum reaction acceleration and signal enhancement and implementation method
Technical Field
The invention relates to the technical field of manufacturing of ion optical devices, in particular to a vortex tube for mass spectrum reaction acceleration and signal enhancement and an implementation method thereof.
Background
The mass spectrum has high specificity, high sensitivity, high analysis speed and certain structural characterization capability, so the mass spectrum is widely applied to the field of reaction monitoring. People follow the reaction process by mass spectrometry, study the reaction kinetics, screen catalysts, and elucidate the reaction mechanism by monitoring reaction intermediates. Electrospray ionization (ESI), Nano-liter electrospray ionization (Nano-ESI) plasma sources have been successful in the field of reaction monitoring. During reaction monitoring, it was found that the reaction that proceeded in the droplets ejected by the ESI plasma source was accelerated. The reaction which originally needs special conditions such as high temperature, high pressure, catalyst and the like in the bulk phase can be slowly carried out, can be carried out in a liquid drop on a millisecond time scale, and does not need some harsh conditions.
However, the conventional reaction monitoring and reaction acceleration are realized by adjusting the distance between the ion source and the mass spectrum sample inlet. When monitoring reaction intermediates, an ion source needs to be close to a mass spectrum injection port to shorten the reaction time so as to monitor as many reaction intermediates as possible. When the reaction needs to be accelerated and the reaction product needs to be monitored, the distance between the ion source and the mass spectrum sample inlet needs to be increased continuously so as to increase the reaction time and generate more products. However, the distance between the ion source and the mass spectrometer inlet cannot be elongated indefinitely. With the continuous increase of the distance, a large amount of ions are lost in the process of being transmitted from the ion source to the mass spectrum sample inlet, so that the signal intensity is reduced. The decrease in signal intensity not only affects the mass spectrum quality, but also results in the absence of signal in some low yield products. Although an ion transfer tube is installed between the ion source and the mass spectrometer inlet to partially solve this problem, the ion transfer tube is generally made of stainless steel, and a tube with a corresponding length needs to be reworked each time the distance between the ion source and the mass spectrometer inlet needs to be adjusted. Furthermore, the laboratory space limitations mean that the length of the ion transfer tube is still very limited. This solution is clearly unsatisfactory. Compared with the ESI ion source, the Nano-ESI ion source has no sheath gas assist, and almost no mass spectrum signal can be detected when the distance from the mass spectrum sample inlet is larger than 15 cm. Even if an ion transport tube is installed between the mass spectrum sample inlet and the ion source, the problem cannot be solved well.
In addition to the above problems, ESI and Nano-ESI plasma sources also suffer from low ionization efficiency caused by slow solvent volatilization rate, low mixing and contact efficiency between reactant ions, and the like in the reaction monitoring and reaction acceleration processes.
Disclosure of Invention
In view of the foregoing analysis, the present invention aims to provide a vortex tube for mass spectrometry reaction acceleration and signal enhancement and a realization method thereof, so as to solve the problems of low ion transmission efficiency and ionization efficiency, low reactant ion mixing contact efficiency and difficult adjustment of reaction time in the reaction monitoring and reaction acceleration processes of the existing mass spectrometry.
The purpose of the invention is mainly realized by the following technical scheme:
in one aspect, the invention provides a vortex tube for enhancing a mass spectrometry response signal, which comprises a sealing tube and a threaded tube with an axial ion channel, wherein the threaded tube is provided with an external thread and is arranged in the sealing tube, and a groove of the external thread is used as a gas channel; the vortex tube is arranged between the ion source and the mass spectrum sample inlet; and the side wall of the sealing pipe is provided with a gas flow inlet for introducing gas.
On the basis of the scheme, the invention is further improved as follows:
further, the threaded pipe is arranged on the side close to the mass spectrum sample inlet.
Further, the airflow inlet is arranged on the sealing tube close to the mass spectrum sample inlet side.
Furthermore, one end of the threaded pipe is flush with one end of the sealing pipe, which is provided with the airflow inlet.
Further, the length of the sealing tube is greater than that of the threaded tube.
Furthermore, the thread pitch of the external thread is 1.5-5 mm.
Further, the difference between the lengths of the sealing tube and the threaded tube is 5-30 mm.
Further, the diameter of the ion channel is 1.0-6.0 mm.
In another aspect, the present invention also provides a method for enhancing a mass spectral signal, comprising the steps of:
step (1): an ion source is arranged at the outlet end of the vortex tube, and a mass spectrum sample inlet is arranged at the inlet end of the vortex tube;
step (2): injecting a sample into an ion source, and applying high voltage, wherein a tip of the ion source generates charged liquid drops; introducing inert gas into the vortex tube through a gas flow inlet on the side wall of the sealing tube;
and (3): forming charged ions in the charged liquid drops in the step (2) in a vortex tube, and enabling the charged ions to enter a mass spectrum through an ion channel of a threaded tube to be detected;
and (4): the flow rate of the inert gas is adjusted to adjust the reaction time of the charged ions in the vortex tube, so as to enhance the mass spectrum response signal of the reaction product or the reaction intermediate.
Further, the high pressure in step (2) is 1000-5000V.
The invention can realize at least one of the following beneficial effects:
(1) according to the embodiment of the invention, by adopting the structural form of the sealing pipe with the built-in threaded pipe and arranging the external thread on the threaded pipe, the air flow which originally flows linearly is in a spiral advancing state in the groove of the external thread. When the gas flow exits the threaded tube, a vortex is formed in the sealed tube and has a certain velocity in the axial direction. Because the gas flow velocity near the ion source is accelerated, the volatilization rate of the solvent in the small liquid drops generated by the ion source is accelerated, so that the ionization efficiency is improved, and the signal of sample ions in the mass spectrum is enhanced.
(2) The vortex created in the sealed tube may allow for more rapid mixing between the reactant ions, thereby increasing the reaction rate.
(3) The vortex generated in the sealed tube can make the mixing between reactant ions more uniform, thereby improving the droplet reaction efficiency.
(4) According to the invention, the length of the sealing pipe is set to be larger than that of the threaded pipe, a certain space can be formed in the sealing pipe and at the position where the threaded pipe is not arranged, airflow flows out of the threaded pipe to form a vortex in the space, and due to the existence of the space, the mixing of reactant ions is quicker and more uniform, and the reaction rate and the reaction efficiency are further improved.
(5) By selecting the proper diameter of the ion channel, controlling the screw pitch and the length difference between the sealing tube and the threaded tube, the mass spectrum signal is improved by about two orders of magnitude after the vortex tube is arranged.
In the invention, the technical schemes can be combined with each other to realize more preferable combination schemes. Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, wherein like reference numerals are used to designate like parts throughout.
FIG. 1 is a schematic structural view of a vortex tube provided in embodiment 1;
FIG. 2 is one of the methods of using the vortex tube provided in embodiment 2;
FIG. 3 is a total ion current chromatogram for analyzing small molecular oleylamine by Nano-ESI-MS with a vortex tube in application example 1;
FIG. 4 is a total ion flow chromatogram for analysis of macromolecular myoglobin by Nano-ESI-MS with vortex tube in application example 1;
FIG. 5 is an extracted ion current chromatogram of a product of a Nano-ESI-MS with a vortex tube for a brain Wen lattice reaction in application example 2;
FIG. 6 is a graph showing the relationship between the normalized signal intensity of the product and the gas flow rate for the brain Wedgelet reaction using the Nano-ESI-MS with vortex tube in application example 2.
Reference numerals:
1-sealing the tube; 2-a threaded pipe; 3-an ion channel; 4-a gas stream inlet; 5-an ion source; 6-mass spectrum sample inlet; 7-vortex gas; 8-high voltage power supply.
Detailed Description
The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, which form a part hereof, and which together with the embodiments of the invention serve to explain the principles of the invention and not to limit its scope.
One embodiment of the invention discloses a vortex tube used between an ion source and a mass spectrum sample inlet, which comprises a sealing tube 1 and a threaded tube 2 with an axial ion channel 3, wherein the threaded tube 2 is provided with external threads and is arranged in the sealing tube 1 and is tightly matched with the sealing tube in a sliding way; the groove of the external thread is used as a gas channel, the vortex tube is arranged between the ion source 5 and the mass spectrum sample inlet 6, the inlet end of the vortex tube is close to the mass spectrum sample inlet 6, and the outlet end of the vortex tube is close to the ion source; the side wall of the sealed tube 1 is provided with a gas flow inlet 4 for introducing gas. Illustratively, the airflow inlet 4 has a diameter of 1-3 mm. The ion channel 3 is used for passing ions, and then the ions enter a mass spectrum to be detected.
Compared with the prior art, the vortex tube provided by the embodiment has the special structure of the external thread, so that the gas flow which originally flows linearly is in a spiral advancing state under the constraint of the external thread. When the gas flow exits the threaded tube, a vortex is formed in the sealed tube and has a certain velocity in the axial direction. Because the gas flow speed near the ion source is accelerated, the droplet solvent generated by the ion source is quickly volatilized, so that the ionization efficiency is improved, and the signal of sample ions in the mass spectrum is enhanced.
Considering that reactant ions generated by the ion source need a certain space to be sufficiently mixed under the action of the vortex, the length of the sealing tube is set to be greater than that of the threaded tube in the embodiment of the present invention. Through the design, can be in the sealed tube, not set up screwed pipe department and form certain space, the air current flows out the screwed pipe and forms the vortex in this space, because the existence in this space, makes the mixture between the reactant ion rapider and even more, not only improves reaction rate, improves reaction efficiency moreover.
Since the amount of the solvent in the charged droplets generated from the tip of the ion source is large and the vortex is generated in the sealed tube near the outlet end, the ion source should be disposed near the outlet end of the vortex tube so that the solvent is rapidly volatilized from the droplets containing a large amount of the solvent by the vortex, thereby improving the ionization efficiency.
Since the threaded tube is disposed near the mass spectrometer inlet, in order to make the gas flow be quickly restricted by the external thread, the gas flow inlet should be disposed on the same side as the threaded tube, i.e., on the side wall of the sealed tube near the mass spectrometer inlet, rather than on the side wall of the sealed tube near the ion source end.
It should be noted that, in the actual use process, when monitoring the reaction intermediate, the reaction time needs to be shortened to monitor the reaction intermediate as much as possible; when the reaction needs to be accelerated and the reaction product needs to be monitored, the reaction time needs to be increased so as to generate more products. Therefore, it is desirable that the response time of the vortex tube be adjustable.
In one aspect, the reaction time can be adjusted by adjusting the gas flow. When longer reaction times are required, or more reaction products are desired, the rate of gas flow into the vortex tube is increased only to slow the rate of ions entering the mass spectrometer, thereby increasing the reaction time. Correspondingly, when the reaction time needs to be shortened so as to monitor the reaction intermediates as much as possible, the flow velocity of the gas entering the vortex tube can be reduced, thereby accelerating the speed of ions entering the mass spectrum and further monitoring the reaction intermediates as much as possible.
Considering that the eddy current is not well formed if the difference between the lengths of the sealing tube and the threaded tube is too large or too small, the present embodiment controls the difference between the lengths to be 5 to 30 mm. Many studies have found that when the difference in length is less than 5mm, there is not enough space for mixing of reactant ions, which affects reaction efficiency and reaction yield. When the length difference is greater than 30mm, the formed vortex disappears in the advancing process due to the long length, and the significance of arranging the vortex tube is lost. The length difference between the sealing tube and the threaded tube is controlled to be 5-30mm, which is beneficial to improving the mass spectrum signal of the reaction product.
The formation of the vortex is mainly due to the existence of the external thread, and the size of the thread pitch has a remarkable influence on the experimental effect. When the pitch is less than 1.5mm, the processing difficulty of the threaded pipe is large, and the cost is obviously increased. When the pitch is larger than 5mm, the airflow speed is too high when the airflow flows out of the threaded pipe, the gas helix is not obvious, and charged ions entering the mass spectrum are unstable, so that the temperature of a detection signal is influenced. The screw pitch is controlled to be 1.5-5mm, and the mass spectrum signal of the reaction product is obviously improved.
It is noted that the diameter of the ion channel also has a significant effect on the improvement of the mass spectrometric detection signal. In experiments, when the diameter of an ion channel is smaller than 1.0mm, the transmission efficiency of ions in the channel is low, and the detection efficiency is influenced; when the diameter of the ion channel is too large, a part of ions cannot enter the mass spectrum sample inlet, and the accuracy of a detection result is affected. Therefore, the diameter of the ion channel is controlled to be 1.0-6.0mm, so that the detection efficiency and the detection result are ensured to be accurate.
Another embodiment of the invention discloses a method for enhancing a mass spectral signal, comprising the steps of:
step (1): the ion source is arranged at the outlet end of the vortex tube, the tip end of the ion source is flush with the outlet of the vortex tube, the mass spectrum sample inlet is arranged at the inlet end of the vortex tube, and the mass spectrum sample inlet is flush with the inlet of the vortex tube;
step (2): injecting a sample into the ion source, and applying high pressure of 1000-; introducing nitrogen into the vortex tube through a gas flow inlet on the side wall of the sealing tube;
and (3): the charged liquid drops in the step (2) enter a vortex tube, under the action of vortex gas, the solvent of the charged liquid drops is volatilized in an accelerated mode to form a series of smaller charged liquid drops, finally a charged ion is formed, and the charged ion enters a mass spectrum through an ion channel of a threaded tube to be detected, so that a mass spectrum response signal is improved;
and (4): the reaction time of charged ions in the vortex tube is adjusted by adjusting the flow rate of nitrogen, and the mass spectrum signal of a reaction product or a reaction intermediate is enhanced according to the requirement.
Example 1
The vortex tube provided by the embodiment comprises a sealing tube and a threaded tube. The total length of the threaded pipe is 15.0mm, the maximum outer diameter is 10.0mm, the thread section is a rectangle with the diameter of 2.0mm multiplied by 1.5mm, and the thread pitch is 3.5 mm. The center of the threaded pipe is provided with an ion channel with the diameter of 4.0 mm. The tube was 30.0mm in length, 10.1mm in inside diameter and 11.0mm in outside diameter, and left a small 2.5mm diameter hole at one end to allow gas to be introduced into the vortex tube. The threaded pipe is sleeved into the sealing pipe, the threaded pipe and the sealing pipe are in tight sliding fit, and one end of the threaded pipe is aligned with one end of the sealing pipe where the small air inlet hole is located. Gas is introduced from the small holes and into the threaded grooves. Under the flow guide effect of the screw thread, the gas advances spirally, after 15mm, the gas breaks away from the screw thread constraint at the end of the screw thread pipe, and a vortex is directly formed in the sealing pipe.
Example 2
This embodiment provides one use of the vortex tube of the present invention. As shown in FIG. 2, the Nano-ESI ion source is placed on the front side of the vortex tube with its tip flush with the vortex tube outlet. The vortex tube is arranged between the ion source and the mass spectrum sample inlet. When the sample is injected and the high voltage of 1000-. The small droplets are subjected to the action of the vortex gas 7, the solvent is rapidly volatilized, and the droplet volume is reduced. The reactants inside the droplet are continuously accumulated on the surface of the droplet, and when the surface tension of the droplet is exceeded, "coulomb explosion" occurs, and the droplet is further changed into a smaller droplet. After several cycles of such processes, one charged ion is finally formed in the vortex tube and finally enters into the mass spectrum to be detected. During the passage of droplets and charged ions through the vortex tube, the vortex gas acts as follows: solvent volatilization is accelerated, and ionization efficiency is improved, so that mass spectrum response signals are improved; the vortex drives sufficient mixing between the reactant droplets/reactant ions; the vortex gas with axial velocity can decelerate ions flying to the mass spectrum, thereby increasing the reaction time between ions, adjusting the size of the vortex gas and further adjusting the reaction time of the ions.
Application example 1
The application example verifies that the vortex tube has the effects of increasing ionization efficiency and improving signal intensity for small molecules and macromolecular substances. FIG. 3 is a total ion flow chromatogram of a Nano-ESI-MS analysis of small molecule oleylamine with a vortex tube. The specific experimental device is shown in FIG. 2. Oleylamine having the molecular formula C18H37N, molecular weight 267, is a typical small molecule compound. The total ion current chromatogram in the graph shows the distribution of high and low signals which are alternately appeared, wherein the gas flow velocity in the vortex tube at the higher signal is 1.5 L.min-1And the airflow at the lower signal is 0. The addition of the vortex gas improves the signal by about two orders of magnitude compared to the state without the vortex gas.
FIG. 4 is a total ion flow chromatogram for analysis of macromolecular myoglobin by Nano-ESI-MS with vortex tube. The specific experimental device is shown in FIG. 2. Myoglobin has a molecular weight of 16700 and is a typical macromolecule. As with small molecules, the total ion current chromatogram in the graph exhibits a distribution of alternating high and low signals, where the vortex tube appears at higher signalsThe flow rate of the gas in the middle-jiao gas is 1.5 L.min-1And the airflow at the lower signal is 0. The addition of the vortex gas improves the signal by about two orders of magnitude compared to the state without the vortex gas.
Application example 2
This example demonstrates the beneficial effect of vortex tubes on droplet reaction acceleration. The model reaction used is shown in FIG. 5. For simplicity, the two reactants are denoted a and B, respectively, and the product is denoted P. The specific experimental apparatus is shown in fig. 2, wherein a reactant a and a reactant B are uniformly mixed in a centrifugal tube, and then injected into a Nano-ESI nozzle, and after high pressure is applied, the reactant a and the reactant B react in the sprayed liquid drops to generate a product P. FIG. 5 bottom is the product [ P + Na ] for this reaction using Nano-ESI-MS equipped with vortex tube]+The extracted ion current chromatogram of (1). The chromatogram of the extracted ion current is distributed in a step shape from left to right, and the eddy current gas flow velocity (unit is L.min) corresponding to each step-1) 0, 0.5, 1.0, ≥ 1.5, 1.0, 0.5 and 0 respectively. As can be seen from fig. 5, the relative intensity of the reaction product P increases as the flow rate of the swirling gas increases. The figure also illustrates the good stability and reproducibility of the device of the invention.
To more clearly and concisely express the relationship between the relative intensity of the signal and the gas flow rate, the normalized (product/reactant) signal intensity is plotted on the ordinate versus the vortex gas flow rate on the abscissa, as shown in FIG. 6. As is clear from the graph in FIG. 6, the normalized signal intensity (product/reaction) gradually increased with increasing gas flow and reached 1.5 L.min at the gas flow rate-1After that, the enhancement effect does not increase.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims (3)

1. A method for enhancing a mass spectral signal, comprising the steps of:
step (1): an ion source is arranged at the outlet end of the vortex tube, and a mass spectrum sample inlet is arranged at the inlet end of the vortex tube;
step (2): injecting a sample into an ion source, and applying high voltage, wherein a tip of the ion source generates charged liquid drops; introducing inert gas into the vortex tube through a gas flow inlet on the side wall of the sealing tube;
and (3): forming charged ions in the charged liquid drops in the step (2) in a vortex tube, and enabling the charged ions to enter a mass spectrum through an ion channel of a threaded tube to be detected;
and (4): the flow velocity of the inert gas is adjusted to adjust the reaction time of the charged ions in the vortex tube, so as to enhance the mass spectrum response signal of the reaction product or the reaction intermediate.
2. The method for enhancing mass spectrometry signals of claim 1, wherein the high pressure in step (2) is 1000-5000V.
3. The method for enhancing mass spectrometry signals of claim 2, wherein the method uses a vortex tube consisting of a sealed tube and a threaded tube with an axial ion channel, the threaded tube having an external thread and being disposed in the sealed tube and being in close sliding fit with the sealed tube, the groove of the external thread serving as a gas channel; the vortex tube is arranged between the ion source and the mass spectrum sample inlet; the side wall of the sealing pipe is provided with an airflow inlet for introducing gas;
the threaded pipe is provided with external threads on the whole length;
the length difference between the sealing pipe and the threaded pipe is 5-30 mm;
the diameter of the ion channel is 4.0-6.0 mm;
the airflow inlet is directly communicated with the groove of the external thread;
the threaded pipe is arranged on the side close to the mass spectrum sample inlet;
the gas flow inlet is arranged on the sealing tube close to the mass spectrum sample inlet side;
one end of the threaded pipe is flush with one end of the sealing pipe, which is provided with the airflow inlet;
the length of the sealing pipe is greater than that of the threaded pipe;
the thread pitch of the external thread is 1.5-5 mm;
the reaction time of the turbine pipe is adjustable;
the outlet of the vortex tube is flush with the tip of the ion source, and the inlet of the vortex tube is flush with the mass spectrum sample inlet.
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CN110726798B (en) * 2019-11-27 2022-04-15 上海华力微电子有限公司 Sample introduction sealing device, gas chromatography-mass spectrometer and chromatographic column replacement method
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