CN210467762U - Microbead electrospray array high-flux analysis device - Google Patents
Microbead electrospray array high-flux analysis device Download PDFInfo
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- CN210467762U CN210467762U CN201921542710.1U CN201921542710U CN210467762U CN 210467762 U CN210467762 U CN 210467762U CN 201921542710 U CN201921542710 U CN 201921542710U CN 210467762 U CN210467762 U CN 210467762U
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- microballon
- flow channel
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- 238000004458 analytical method Methods 0.000 title claims abstract description 30
- 239000011325 microbead Substances 0.000 title claims description 39
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 238000001819 mass spectrum Methods 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims description 11
- 239000004020 conductor Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000012811 non-conductive material Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 abstract description 11
- 230000005611 electricity Effects 0.000 abstract description 10
- 230000004907 flux Effects 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 44
- 150000002500 ions Chemical class 0.000 description 11
- 238000000034 method Methods 0.000 description 8
- 238000004949 mass spectrometry Methods 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 239000012488 sample solution Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000000688 desorption electrospray ionisation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 238000000132 electrospray ionisation Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229960001699 ofloxacin Drugs 0.000 description 3
- -1 reserpine compound Chemical class 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- XMAYWYJOQHXEEK-OZXSUGGESA-N (2R,4S)-ketoconazole Chemical compound C1CN(C(=O)C)CCN1C(C=C1)=CC=C1OC[C@@H]1O[C@@](CN2C=NC=C2)(C=2C(=CC(Cl)=CC=2)Cl)OC1 XMAYWYJOQHXEEK-OZXSUGGESA-N 0.000 description 2
- DNXIKVLOVZVMQF-UHFFFAOYSA-N (3beta,16beta,17alpha,18beta,20alpha)-17-hydroxy-11-methoxy-18-[(3,4,5-trimethoxybenzoyl)oxy]-yohimban-16-carboxylic acid, methyl ester Natural products C1C2CN3CCC(C4=CC=C(OC)C=C4N4)=C4C3CC2C(C(=O)OC)C(O)C1OC(=O)C1=CC(OC)=C(OC)C(OC)=C1 DNXIKVLOVZVMQF-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- GSDSWSVVBLHKDQ-UHFFFAOYSA-N 9-fluoro-3-methyl-10-(4-methylpiperazin-1-yl)-7-oxo-2,3-dihydro-7H-[1,4]oxazino[2,3,4-ij]quinoline-6-carboxylic acid Chemical compound FC1=CC(C(C(C(O)=O)=C2)=O)=C3N2C(C)COC3=C1N1CCN(C)CC1 GSDSWSVVBLHKDQ-UHFFFAOYSA-N 0.000 description 2
- LCQMZZCPPSWADO-UHFFFAOYSA-N Reserpilin Natural products COC(=O)C1COCC2CN3CCc4c([nH]c5cc(OC)c(OC)cc45)C3CC12 LCQMZZCPPSWADO-UHFFFAOYSA-N 0.000 description 2
- QEVHRUUCFGRFIF-SFWBKIHZSA-N Reserpine Natural products O=C(OC)[C@@H]1[C@H](OC)[C@H](OC(=O)c2cc(OC)c(OC)c(OC)c2)C[C@H]2[C@@H]1C[C@H]1N(C2)CCc2c3c([nH]c12)cc(OC)cc3 QEVHRUUCFGRFIF-SFWBKIHZSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 229960004125 ketoconazole Drugs 0.000 description 2
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000002674 ointment Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 229960003147 reserpine Drugs 0.000 description 2
- MDMGHDFNKNZPAU-UHFFFAOYSA-N roserpine Natural products C1C2CN3CCC(C4=CC=C(OC)C=C4N4)=C4C3CC2C(OC(C)=O)C(OC)C1OC(=O)C1=CC(OC)=C(OC)C(OC)=C1 MDMGHDFNKNZPAU-UHFFFAOYSA-N 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- CYDMQBQPVICBEU-UHFFFAOYSA-N chlorotetracycline Natural products C1=CC(Cl)=C2C(O)(C)C3CC4C(N(C)C)C(O)=C(C(N)=O)C(=O)C4(O)C(O)=C3C(=O)C2=C1O CYDMQBQPVICBEU-UHFFFAOYSA-N 0.000 description 1
- 229960004475 chlortetracycline Drugs 0.000 description 1
- 235000019365 chlortetracycline Nutrition 0.000 description 1
- BLEBFDYUDVZRFG-UHFFFAOYSA-N dichloromethane;propan-2-ol Chemical compound ClCCl.CC(C)O BLEBFDYUDVZRFG-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000007787 electrohydrodynamic spraying Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005040 ion trap Methods 0.000 description 1
- 238000000752 ionisation method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- BJOIZNZVOZKDIG-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C([C]5C=CC(OC)=CC5=N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 BJOIZNZVOZKDIG-MDEJGZGSSA-N 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
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Abstract
The utility model discloses a microballon electricity spraying array high flux analysis device, including high-pressure contact point, high-pressure connecting wire, introduction port, liquid flow channel and electricity spraying microballon, high-pressure connecting wire both ends link to each other with high-pressure contact point and introduction port respectively, the introduction port links to each other with liquid flow channel, liquid flow channel is direct hollow structure, the electricity spraying microballon inlays at liquid flow channel's end, electricity spraying microballon front end is towards mass spectrum entry channel. The utility model discloses accessible control high voltage electrode is connected with high voltage contact to thereby make high voltage contact electrified make introduction port and liquid flow path electrified, finally make the sample by ionization and mass spectrum detection in proper order, realized quick, high flux and the controllable analysis of sample, have that sample consumption is little, degree of automation is high, low cost and need characteristics such as regulating parameter is few.
Description
Technical Field
The utility model relates to a mass spectrometry technical field, especially a microballon electric spray array high flux analysis device.
Background
The ion source is a key component of the mass spectrometer, and the ionization method of the ion source directly affects the analysis state, the analysis speed, the operation complexity, the ionization efficiency, the analysis cost and the like of a sample. The existing paper spray high-throughput analysis device utilizes a paper tape as a sample carrier, different samples are spotted in different areas of the paper tape, the samples are analyzed by a method of loading high voltage on the paper tape and eluting the samples in front of an ion inlet by using a solvent, and the sample spots are replaced by moving the paper tape. The method can realize automatic batch sample introduction of mass spectra to a certain extent, but the paper tape sample loading has the problems of easy sample diffusion and low analysis speed. Furthermore, the paper tape can also adsorb the sample, causing a loss of analytical sensitivity. In recent years, a batch mass spectrometry sample introduction method based on desorption electrospray ionization technology is also studied, however, although the method adopting desorption electrospray ionization technology can solve the analysis problem of solid samples, the liquid samples are easily blown away by desorption gas flow, so that the embarrassment that the liquid samples are difficult to analyze is caused. In addition, the desorption electrospray ionization technology has poor desorption effect on the large polar compounds, and is not suitable for analysis of the large polar compounds. In addition, high-throughput analysis integrated on a chip has also been reported, but the chip is expensive and is mainly used for analysis of liquid samples. In addition, the chip pipeline is thin, and the flow control of liquid is also complex.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome prior art's shortcoming, provide a microballon electric spray array high flux analytical equipment.
The utility model aims at realizing through the following technical scheme that a microballon electricity spraying array high flux analysis device, including high pressure contact point, high-pressure connecting wire, introduction port, liquid flow channel and electricity spraying microballon, high pressure connecting wire both ends link to each other with high pressure contact point and introduction port respectively, the introduction port links to each other with liquid flow channel, liquid flow channel is direct hollow structure, electricity spraying microballon inlays the end at liquid flow channel, electricity spraying microballon front end is towards mass spectrum entry path, contained angle α between the axis of electricity spraying microballon and the axis of mass spectrum entry path, there are horizontal distance d and vertical distance h between the front end of electricity spraying microballon and the mass spectrum entry path.
Preferably, the microbead electrospray array high-flux analysis device further comprises a high-voltage power supply, and the high-voltage power supply is connected with the high-voltage contact point through a high-voltage electrode.
Preferably, the high-voltage connecting line and the sample inlet are both made of conductive materials.
Preferably, the liquid flow channel is an electrically conductive metal outer wall with a length of 10mm to 50cm and an internal hollow diameter of 25 μm to 0.5 cm.
Preferably, the electrospray micro-beads are hollow or solid spherical or sphere-like structures, are made of conductive materials or non-conductive materials, and have a diameter R <5 mm.
Preferably, the included angle α ranges from 90 ° to 270 °.
Preferably, the horizontal distance d is 0.5-10 mm, and the vertical distance h is 0-10 mm.
Preferably, the sample comprises a solid, liquid, semi-solid form sample.
The utility model has the advantages of it is following: the connection of the high-voltage electrode and the high-voltage contact point is controlled, so that the high-voltage contact point is electrified, the sample inlet and the liquid flow channel are electrified, and finally, the sample is sequentially ionized and detected by mass spectrometry. The utility model discloses a quick, high flux and the programmed analysis of sample have that the sample consumes advantages such as little, degree of automation is high, low cost and need the accommodate parameter few.
Drawings
Fig. 1 is a schematic structural view of the present invention;
FIG. 2 is a mass spectrum of example 1 of the present invention;
fig. 3 is a mass spectrum diagram of embodiment 2 of the present invention;
fig. 4 is a mass spectrum diagram of embodiment 3 of the present invention;
in the figure, 1-high voltage contact point, 2-high voltage connecting line, 3-sample inlet, 4-liquid flow channel, 5-electrospray microbead and 6-mass spectrum inlet channel.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the intended advantageous objects of the present invention, the following detailed description of the embodiments, structures, features and effects according to the present invention will be made with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" may not necessarily refer to the same embodiment, and furthermore, particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments:
as shown in fig. 1, the microbead electrospray array high-throughput analysis device is characterized by comprising a high-voltage contact point 1, a high-voltage connecting line 2, a sample inlet 3, a liquid flow channel 4 and electrospray microbeads 5, wherein two ends of the high-voltage connecting line 2 are respectively connected with the high-voltage contact point 1 and the sample inlet 3, the sample inlet 3 is connected with the liquid flow channel 4, the liquid flow channel 4 is of a straight-through hollow structure, the electrospray microbeads 5 are embedded at the tail end of the liquid flow channel 4, the front ends of the electrospray microbeads face a mass spectrum inlet channel 6, an included angle α is formed between the axis of the electrospray microbeads 5 and the axis of the mass spectrum inlet channel 6, and a horizontal distance d and a vertical distance h are formed between the front ends of the electrospray microbeads 5 and the mass spectrum inlet channel 6.
As an alternative embodiment, the microbead electrospray array high-throughput analysis device further comprises a high-voltage power supply, and the high-voltage power supply is connected with the high-voltage contact point 1 through a high-voltage electrode.
In an alternative embodiment, the high voltage connection line 2 and the injection port 3 are both made of conductive materials.
In an alternative embodiment, the liquid flow channel 4 is an electrically conductive metal outer wall having a length of 10mm to 50cm and an internal hollow diameter of 25 μm to 0.5 cm.
In an alternative embodiment, the electrospray micro-beads 5 are hollow or solid spherical or spheroidal structures, and are made of conductive materials or non-conductive materials, and the diameter R of the electrospray micro-beads is less than 5 mm.
In an alternative embodiment, the included angle α is in the range of 90 ° to 270 °.
As an optional implementation mode, the horizontal distance d is 0.5-10 mm, and the vertical distance h is 0-10 mm.
The method for the bead electrospray array high-throughput analysis device to be used for high-throughput analysis comprises the following steps:
s1, directly adding a sample into the liquid flow channel 4 through the sample inlet 3 or loading the sample into the electrospray microbead 5 in a contact loading mode;
s2, switching on a high-voltage power supply, and applying a high-voltage field to the electrospray micro-beads 5 through the high-voltage contact point 1 by the high-voltage power supply, wherein the voltage is-8000V;
s3, introducing an elution-spraying solvent into the liquid flow channel 4 through the sample inlet 3, eluting and ionizing the sample of the liquid flow channel 4 or the electrospray microbead 5, and finally performing mass spectrometry by the mass spectrometer 6.
In an alternative embodiment, the sample comprises a solid, liquid, or semi-solid form sample and the mass spectrometer comprises a triple quadrupole mass spectrometer, a time-of-flight mass spectrometer, an ion trap mass spectrometer, or an Orbitrap mass spectrometer.
In alternative embodiments, the elution-spray solvent comprises an acidic, neutral or basic methanol-water system, an acidic, neutral or basic acetonitrile-water system, or a dichloromethane-isopropanol system.
Example 1
And analyzing the liquid sample, wherein the selected sample solution to be detected is a reserpine solution with the concentration of 1 mu M.
The method comprises the following steps of introducing a sample into a liquid flow channel 4, wherein the length of the sample is 11mm, the inner diameter of the sample is 2mm, the sample is made of a carbon steel material and is in a conical straight-through hollow structure, an electrospray microbead 5 is a tungsten carbide solid sphere, the radius r of the electrospray microbead is 0.5 mm, the electrospray microbead is embedded into the front end of a microspherical base, the horizontal distance d between the electrospray microbead 5 and a mass spectrum inlet channel 6 is 2mm, the vertical distance h is 0mm, and the included angle α between the axis of the electrospray microbead 5 and the axis of the mass spectrum inlet channel 6:
a.5 muL solution is filled into a liquid flow channel;
B. enabling methanol to enter a sample inlet 3 and then enter a liquid flow channel 4 through a syringe pump, wherein the flow rate is 5 muL/min;
C. a high-voltage power supply is connected, and a high-voltage electric field is applied to the electrospray micro-beads 5 through a high-voltage contact point, wherein the voltage is + 3000V;
D. when the sample solution to be detected flows to the front end of the electrospray microbead 5, electrospray ionization is carried out to form sample ions, the sample ions enter the mass spectrum inlet channel 6, and mass spectrum analysis is carried out by a mass spectrometer.
As shown in FIG. 2, the results of mass spectrometry showed that the reserpine compound gave good abundance of [ M + H ]]+Peak of mass to charge ratio ofm/z609. The signal intensity is 1.88 × 107。
Example 2
And (4) analyzing the solid sample, wherein the selected sample to be detected is the ofloxacin capsule.
The ion source of mass spectrograph does the utility model provides an electrospray mass spectrum device based on microballon, the device parameter with the utility model discloses the parameter among the embodiment 1 is the same. The method specifically comprises the following steps:
A. filling ofloxacin capsule powder into a liquid flowing chamber, and pumping a methanol water solution (volume ratio is 1: 1) containing 0.1% formic acid through a sample inlet by a syringe pump, wherein the flow rate is 5 uL/min;
B. a high-voltage power supply is connected, and a high-voltage electric field is applied to the electrospray micro-beads 5 through the high-voltage contact point 1 by the high-voltage power supply, wherein the voltage is + 3000V;
C. when the sample solution to be detected flows to the front end of the electrospray microbead 5, electrospray ionization is carried out to form sample ions, the sample ions enter the mass spectrum inlet channel 6, and mass spectrum analysis is carried out by a mass spectrometer.
As shown in FIG. 3, the results of mass spectrometry showed that the ofloxacin compound gave good abundance of [ M + H ]]+Peaks of mass to charge ratio ofm/z362. The signal intensity is 3.15 multiplied by 107。
Example 3
And analyzing the semi-solid sample, wherein the selected sample to be detected is ketoconazole ointment.
The ion source of mass spectrograph does the utility model provides an electrospray mass spectrum device based on microballon, the device parameter with the utility model discloses the parameter among the embodiment 1 is the same. The method specifically comprises the following steps:
A. dipping a small amount of ketoconazole ointment by using the electrospraying microbeads 5, and pumping methanol aqueous solution (volume ratio is 1: 1) containing 0.1% formic acid through a sample inlet by a syringe pump, wherein the flow rate is 5 uL/min;
B. a high-voltage power supply is connected, and a high-voltage electric field is applied to the electrospray micro-beads 5 through the high-voltage contact point 3 by the high-voltage power supply, wherein the voltage is + 3000V;
C. when the sample solution to be detected flows to the front end of the electrospray microbead 5, electrospray ionization is carried out to form sample ions, the sample ions enter the mass spectrum inlet channel 6, and mass spectrum analysis is carried out by a mass spectrometer.
As shown in FIG. 4, the results of mass spectrometry showed that the aureomycin compound gave good abundance of [ M + H ]]+Peak of mass to charge ratio ofm/z531 signal intensity of 7.00 × 107。
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications without inventive contribution to the present embodiment as required after reading the present specification, as long as they are protected by patent laws within the scope of the claims of the present invention.
Claims (9)
1. The utility model provides a microballon electrospray array high throughput analysis device which characterized in that includes the base plate and distributes a plurality of contact points (1), connecting wire (2) and introduction port (3) on the base plate, connecting wire (2) both ends link to each other with contact point (1) and introduction port (3) respectively, still include liquid flow channel (4) and microballon (5), the other end and liquid flow channel (4) of introduction port (3) link to each other, liquid flow channel (4) are through hollow structure, microballon (5) are inlayed at the end of liquid flow channel (4), the microballon front end is towards mass spectrum entry passageway (6), contained angle α between the axis of microballon (5) and the axis of mass spectrum entry passageway (6), there are horizontal distance d and vertical distance h between the front end of microballon (5) and mass spectrum entry passageway (6).
2. The microbead electrospray array high throughput analysis device of claim 1, wherein: the micro-beads (5) are electrospray micro-beads.
3. The microbead electrospray array high throughput analysis device of claim 1, wherein: the high-voltage power supply is connected with the contact point (1) through a high-voltage electrode.
4. The microbead electrospray array high throughput analysis device of claim 3, wherein: an electric control switch is arranged in a connecting loop of the high-voltage power supply and the contact point (1).
5. The microbead electrospray array high throughput analysis device of claim 1, wherein: the connecting wire (2) and the sample inlet (3) are made of conductive materials.
6. The microbead electrospray array high throughput analysis device of claim 1, wherein: the liquid flow channel (4) is a conductive metal outer wall, the length of the liquid flow channel is 10 mm-50 cm, and the diameter of the inner hollow part is 25 mu m-0.5 cm.
7. The microbead electrospray array high throughput analysis device of claim 1, wherein: the micro-beads (5) are in hollow or solid spherical or sphere-like structures, are made of conductive materials or non-conductive materials, and have the diameter R <5 mm.
8. The device for high throughput analysis according to claim 1, wherein the included angle α is in the range of 90-270 °.
9. The microbead electrospray array high throughput analysis device of claim 1, wherein: the horizontal distance d is 0.5-10 mm, and the vertical distance h is 0-10 mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921542710.1U CN210467762U (en) | 2019-09-17 | 2019-09-17 | Microbead electrospray array high-flux analysis device |
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| CN201921542710.1U CN210467762U (en) | 2019-09-17 | 2019-09-17 | Microbead electrospray array high-flux analysis device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110491768A (en) * | 2019-09-17 | 2019-11-22 | 中国科学院成都生物研究所 | A kind of microballon electron spray array high throughput analysis device and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110491768A (en) * | 2019-09-17 | 2019-11-22 | 中国科学院成都生物研究所 | A kind of microballon electron spray array high throughput analysis device and method |
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