CN206225322U - ESI ion source devices, mass spectrograph and liquid chromatography mass combined instrument - Google Patents

ESI ion source devices, mass spectrograph and liquid chromatography mass combined instrument Download PDF

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Publication number
CN206225322U
CN206225322U CN201621229362.9U CN201621229362U CN206225322U CN 206225322 U CN206225322 U CN 206225322U CN 201621229362 U CN201621229362 U CN 201621229362U CN 206225322 U CN206225322 U CN 206225322U
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ion source
heating
metal capillary
metal
source devices
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CN201621229362.9U
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田琴琴
莫婷
邹星
黄保
朱辉
李辉
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Guangzhou Hexin Instrument Co Ltd
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Guangzhou Hexin Instrument Co Ltd
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Abstract

The utility model is related to a kind of ESI ion source devices for being applied to mass spectrograph and liquid chromatography mass combined instrument.The ESI ion source devices include housing, atomizer and heat auxiliary pneumatic module, the metal sleeve is used to electrically connect with power supply unit so that the metal capillary is powered, and end where the gas outlet of the auxiliary pneumatic module of heating is stretched into the ion source chamber room for being directed at the spraying from atomizer ejection.The ESI ion source devices that the utility model is related to, by rationally setting metal capillary and metal sleeve, the problem that quartz capillary can be overcome to be collapsed using syringe needle for a long time, high-tension electricity can be applied directly on metal capillary, and sample is more easy to powered;Meanwhile, the auxiliary pneumatic module of heating can freely adjust the distance and the heating-up temperature to air-flow of gas outlet and spraying as needed, sample can be made fully quickly to remove solvent.

Description

ESI ion source devices, mass spectrograph and liquid chromatography mass combined instrument
Technical field
The utility model is related to testing equipment field, more particularly to a kind of ESI ion source devices, mass spectrograph and liquid phase color Spectrum GC-MS.
Background technology
Liquid chromatography mass combined instrument (liquid Chromatograph Mass Spectrometer), abbreviation LC-MS, LC-MS is Analysis of Organic Substances laboratory, medicine, Food Inspection room, the essential analysis of department such as production process control, quality inspection Instrument, it combines liquid chromatograph and efficiently separates thermally labile, the ability of higher-boiling compound and the very strong component of mass spectrograph Identification capacity, is a kind of effective means for separating the complicated organic mixture of analysis.Liquid chromatogram (LC) can effectively will be organic Each composition thing of thing testing sample is separated, and mass spectrum (MS) can obtain organic matter to the analysis one by one of the organic matter that separates Molecular weight, structure and concentration information.Liquid chromatogram and mass spectrum connection being capable of precise Identification and quantitative picture cell and Tissue Lysis Minor compound in the complex sample matrix such as liquid, blood, blood plasma, urine and oral fluid.
High performance liquid chromatography mass spectrometer system has unique analysis detection advantage:Analyze speed is fast, and required sample size is few, spirit Sensitivity is high, and accuracy is high, high resolution, target analytes can be carried out qualitative and quantitative etc..However, liquid chromatograph and matter The online key of spectrometer is to be applicable the exploitation of interface and ESI ion guns, and needs to ensure that sample fraction has to enter into vacuum system Preceding removal solvent.
ESI (Eletrospray Ionization, electron spray) is a kind of conventional atmospheric pressure ionization method, is a kind of soft Ionization technique.ESI Soft ionization techniques and mass spectrographic perfect adaptation solve the measure and liquid chromatogram and matter of big quality molecules Two big challenge problem associated with spectrum.ESI-MS has evolved into a kind of general mass-spectrometric technique, the analysis application neck that it is covered Domain is extremely extensive.Multi-charge ionization due to ESI, the high efficiency to the ionization of some polar compounds (are approached to protein And the characteristic such as soft ionization 100%) so that ESI-MS decomposed in analysis polar compound (including the ion in solution), easily and Macromolecule compound aspect turns into one of maximally effective instrument.
Traditional ESI ion guns are easy using syringe needle for a long time when high-tension electricity is supplied frequently with quartz capillary nozzle needle Collapse, and sample does not allow easily ionizable.In addition, the optimal sample introduction flux of traditional ESI ion guns is 1~10uL/min, it is impossible to full Sufficient liquid chromatogram is required with the high flux sample detection of mass spectrometry.Due to sample flow it is larger when, sample goes solvent effect It is not good, cause detection sensitivity low.
Utility model content
Based on this, it is necessary to provide a kind of ESI ion source devices, mass spectrum for improving sample ionization effect and going solvent effect Instrument and liquid chromatography mass combined instrument.
A kind of ESI ion source devices, including housing, atomizer and the auxiliary pneumatic module of heating;
There is ion source chamber in the housing;
The atomizer includes metal capillary and metal sleeve;Stretch into the ion gun in one end of the metal capillary In chamber, the other end is used for sample introduction;The metal sleeve is set in the outside of the metal capillary, and the metal sleeve wears In on the housing, the metal sleeve is used to be electrically connected with power supply unit so that the metal capillary is powered, the metal Sheath gas passage is formed between sleeve and the metal capillary, the sheath gas passage makes to be sprayed from the metal capillary by supply The state of ionization sample atomization for going out sprays;
The auxiliary pneumatic module at least two of heating, heats auxiliary pneumatic module and is symmetrically located in the housing described at least two On, end where the gas outlet of the auxiliary pneumatic module of heating is stretched into the ion source chamber room for being aligned from atomizer spray The spraying for going out.
Wherein in one embodiment, the auxiliary pneumatic module of heating includes that heating muff, ceramic bead, heating rod, temperature are passed Sensor and fixes sleeve;
The heating muff is provided with air inlet and gas outlet;The ceramic bead is filled in the heating muff;It is described to add Hot pin and the temperature sensor are each passed through end where the air inlet of the heating muff and stretch in the heating muff;
The fixes sleeve coordinates with the heating muff to be installed, and the fixes sleeve wears on the housing and makes described Stretch into the ion source chamber room at end where the gas outlet of heating muff.
Wherein in one embodiment, the folder where the gas outlet of the heating muff between end and the metal capillary Angle is 55 ° -65 °.
Wherein in one embodiment, also including fixed cover;
The fixed cover is installed on the atomizer, and the fixed cover is fixedly connected with the housing, the fixed cover Gas passage is inside provided with to be supplied for connection source of the gas and to the sheath gas passage.
Wherein in one embodiment, position adjustments knob is additionally provided with the fixed cover, the position adjustments knob is used In the position for adjusting the metal capillary.
Wherein in one embodiment, the position adjustments knob has 2 groups, and position adjustments knob is used for described in one of which The upper-lower position of the metal capillary is adjusted, position adjustments knob described in another group is used to adjust a left side for the metal capillary Right position.
Wherein in one embodiment, the housing is provided with observation window;The bottom of the ion source chamber is provided with discharge Mouthful.
A kind of mass spectrograph, including spectrometer body, connecting plate and above-mentioned ESI ion source devices;
The spectrometer body includes mass spectrometer, and the mass spectrometer has ion sampling end, and the ion is adopted Sample end is stretched in the ion source chamber room through the through hole of the connecting plate, the connecting plate respectively with the spectrometer body It is fixedly connected with the housing.
Wherein in one embodiment, the mass spectrograph also includes sealing ring, and the sealing ring is arranged the ion and uses For the sealing ion source chamber on end.
A kind of liquid chromatography mass combined instrument, including liquid chromatograph and above-mentioned mass spectrograph, the liquid chromatograph go out Sample mouthful is connected with the inlet of the metal capillary.
Above-mentioned ESI ion source devices include housing, atomizer and heat auxiliary pneumatic module;There is ion source chamber in the housing Room;The atomizer includes metal capillary and metal sleeve, and the metal sleeve is used to be electrically connected with power supply unit so that institute State metal capillary powered, sheath gas passage is formed between the metal sleeve and the metal capillary, the sheath gas passage leads to Crossing supply makes the state of ionization sample sprayed from the metal capillary be atomized ejection;Where the gas outlet of the auxiliary pneumatic module of heating Stretch into the ion source chamber room for being directed at the spraying sprayed from the atomizer at end.The ESI that the utility model is related to from Source arrangement is used for mass spectrograph, by rationally setting metal capillary and metal sleeve, can overcome quartz capillary for a long time Collapsed using syringe needle and can not long-time high-temperature baking problem, high-tension electricity can be applied directly on metal capillary, and sample is more easy to Powered, atomizing effect more preferably, is operated safer.The auxiliary pneumatic module of heating can freely adjust gas outlet with spraying as needed Distance and to the heating-up temperature of air-flow, at least two beam high temperature gas flows be then oriented more at simultaneously spray, can fill sample Divide quick removal solvent, meet high flux detection and require.
Further, the auxiliary pneumatic module of heating described in the utility model, middle filling ceramic bead, Neng Gouzeng in heating muff Atmospheric heated surface area, the efficiency of heating surface is high, air-flow can be heated into 500~600 DEG C of high temperature, effectively molten in removal sample Agent.With the angle of metal capillary at 55 ° -65 °, the high temperature gas flow of ejection can at end where the gas outlet of the heating muff Increase the amount that charged particle enters sampling heap, improve detection sensitivity.
Comprising above-mentioned ESI ion source devices mass spectrograph and liquid chromatography mass combined instrument can improve sample ionization effect and Solvent removal effect, improves the detection sensitivity of mass analyzer.
Brief description of the drawings
Fig. 1 is the schematic diagram of the ESI ionization source devices of an embodiment;
Fig. 2 is the partial enlargement structural representation of atomizer and fixed cover in Fig. 1.
Specific embodiment
For the ease of understanding the utility model, the utility model is more fully retouched below with reference to relevant drawings State.Preferred embodiment of the present utility model is given in accompanying drawing.But, the utility model can come real in many different forms It is existing, however it is not limited to embodiment described herein.On the contrary, the purpose for providing these embodiments is made to public affairs of the present utility model The understanding for opening content is more thorough comprehensive.
It should be noted that when element is referred to as " being fixed on " another element, it can directly on another element Or can also there is element placed in the middle.When an element is considered as " connection " another element, it can be directly connected to To another element or may be simultaneously present centering elements.
It is intended merely to describe the mesh of specific embodiment in term used in the description of the present utility model herein , it is not intended that in limitation the utility model.
Incorporated by reference to Fig. 1 to Fig. 2, the ESI ion source devices 10 of an embodiment, including housing 100, atomizer 200, heat it is auxiliary Pneumatic module 300 and fixed cover 400.
There is ion source chamber 101 in housing 100.In the present embodiment mode, specifically, the top of housing 100 is provided with Observation window, in Real Time Observation ion source chamber 101.In addition, the bottom center of ion source chamber 101 is provided with outlet, use Waste gas and waste liquid during sample test is discharged, belong to preferred technical scheme.In other embodiments, outlet also may be used To be located at the other positions of ion source chamber as needed.
Atomizer 200 includes metal capillary 210 and metal sleeve 220.
One end of metal capillary 210 is stretched into ion source chamber 101, and the other end is connected for entering by with peek pipes Sample.Metal capillary 210 is stainless steel capillary, and in the present embodiment, specifically, length is 93mm, and internal diameter is 0.5mm. In other embodiment, the size of metal capillary 210 can do accommodation.
Metal sleeve 220 is set in the outside of metal capillary 210, and metal sleeve 220 is arranged on housing 100, metal Sleeve 220 is used to be electrically connected with power supply unit so that metal capillary 210 is powered, metal sleeve 220 and metal capillary 210 it Between formed sheath gas passage, sheath gas passage by supply make from metal capillary 210 spray state of ionization sample be atomized spray.Metal Capillary 210 can not only pass through fluid sample, and can make fluid sample ionize spray and with sheath gas passage supply Gases at high pressure fusion makes the atomization of state of ionization droplet sample spray and solvent is volatilized.
Auxiliary pneumatic module 300 at least two is heated, at least two auxiliary pneumatic modules 300 of heating are symmetrically located on housing 100, Stretch into ion source chamber 101 for being directed at the spray sprayed from atomizer 200 at end where heating the gas outlet of auxiliary pneumatic module 300 Mist.In the present embodiment mode, two auxiliary pneumatic modules 300 of heating are symmetrically located on housing 100 and positioned at the both sides of atomizer. Symmetric double pipeline is set, and two beam high temperature nitrogen air-flows are then oriented more at spraying simultaneously, ensure that sample spraying fully removal Solvent.
In the present embodiment, heating auxiliary pneumatic module 300 includes heating muff, ceramic bead, heating rod, temperature sensor and consolidates Determine sleeve, it is easy to assembly.
Heating muff is provided with air inlet and gas outlet.Ceramic bead is filled in heating muff.Heating rod and temperature sensor It is each passed through end where the air inlet of heating muff and stretches in heating muff.Fixes sleeve coordinates with heating muff to be installed, Fixes sleeve wears on housing and the gas outlet place end of heating muff is stretched into ion source chamber room.Filled out in the heating muff Ceramic bead is filled, gas heated surface area can be increased, the efficiency of heating surface is high, air-flow can be heated to 500~600 DEG C of high temperature, effectively Solvent in removal sample.In the present embodiment mode, where the gas outlet of heating muff between end and metal capillary 210 Angle is 60 °, and preferred angular range is 55 ° -65 °, and charged ion can be made to be more easily aligned mass spectrum mouthful, is improved mass spectrometric Detection sensitivity.
Fixed cover 400 is installed on atomizer 200, and fixed cover 400 is fixedly connected with housing 100, is provided with fixed cover 400 Gas passage is supplied for connection source of the gas and to sheath gas passage.Source of the gas is source nitrogen, for sheath gas passage and the auxiliary gas of heating Supply high pressure nitrogen in heating muff in component 300.
In the present embodiment, position adjustments knob (unmarked in figure), position adjustments knob are additionally provided with fixed cover 400 For being accurately positioned and the position of metal capillary 210 is adjusted, to meet metal capillary 210 to the distance needs of mass spectrum mouthful. Position adjustments knob has 2 groups, and one of which position adjustments knob is used to adjust the upper-lower position of metal capillary 210, another group Position adjustments knob is used to adjust the right position of metal capillary 210.In other embodiments, position adjustments knob may be used also Set with the actual conditions according to assembling, not limited to this.
The ESI ion source devices 10 that the utility model is related to are used for mass spectrograph, by rationally setting the He of metal capillary 210 Metal sleeve 220, can overcome quartz capillary collapsed using syringe needle for a long time and can not long-time high-temperature baking problem, it is high Piezoelectricity can be applied directly on metal capillary 210, sample be more easy to it is powered, atomizing effect more preferably, operate it is safer.Heat auxiliary gas group Part 300 can freely adjust the distance and the heating-up temperature to air-flow of gas outlet and spraying, at least two beam High Temperature Gas as needed Stream is then oriented more at spraying simultaneously, and sample can be made fully quickly to remove solvent, meets high flux detection and requires.
A kind of mass spectrograph, including spectrometer body, connecting plate 21 and ESI ion source devices 10.
Spectrometer body includes mass spectrometer, and mass spectrometer has ion sampling end, and ion sampling end passes through connection The through hole of plate 21 is stretched in ion source chamber 101, and connecting plate 21 is fixedly connected with spectrometer body and housing 100 respectively.
Mass spectrograph also includes sealing ring 22, and sealing ring 22 is arranged ion and uses on end for sealing ion source chamber 101.
A kind of liquid chromatography mass combined instrument, including liquid chromatograph and above-mentioned mass spectrograph, the outlet of liquid chromatograph Inlet with metal capillary 210 is connected.
Mass spectrograph comprising ESI ion source devices 10 and liquid chromatography mass combined instrument can improve sample ionization effect and Solvent removal effect, improves the detection sensitivity of mass analyzer.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses several embodiments of the present utility model, and its description is more specific and detailed, But therefore can not be interpreted as the limitation to utility model patent scope.It should be pointed out that for the common skill of this area For art personnel, without departing from the concept of the premise utility, various modifications and improvements can be made, these are belonged to Protection domain of the present utility model.Therefore, the protection domain of the utility model patent should be determined by the appended claims.

Claims (10)

1. a kind of ESI ion source devices, it is characterised in that including housing, atomizer and heat auxiliary pneumatic module;
There is ion source chamber in the housing;
The atomizer includes metal capillary and metal sleeve;Stretch into the ion source chamber in one end of the metal capillary Interior, the other end is used for sample introduction;The metal sleeve is set in the outside of the metal capillary, and the metal sleeve is arranged in institute State on housing, the metal sleeve is used to be electrically connected with power supply unit so that the metal capillary is powered, the metal sleeve Sheath gas passage is formed and the metal capillary between, the sheath gas passage makes what is sprayed from the metal capillary by supply The atomization of state of ionization sample sprays;
The auxiliary pneumatic module at least two of heating, heats auxiliary pneumatic module and symmetrically wears on the housing described at least two, Stretch into the ion source chamber room for being aligned from atomizer ejection at end where the gas outlet of the auxiliary pneumatic module of heating Spraying.
2. ESI ion source devices as claimed in claim 1, it is characterised in that the auxiliary pneumatic module of heating include heating muff, Ceramic bead, heating rod, temperature sensor and fixes sleeve;
The heating muff is provided with air inlet and gas outlet;The ceramic bead is filled in the heating muff;The heating rod End where the air inlet of the heating muff is each passed through with the temperature sensor and stretch in the heating muff;
The fixes sleeve coordinates with the heating muff to be installed, and the fixes sleeve wears on the housing and makes the heating Stretch into the ion source chamber room at end where the gas outlet of sleeve.
3. ESI ion source devices as claimed in claim 2, it is characterised in that end where the gas outlet of the heating muff with Angle between the metal capillary is 55 ° -65 °.
4. ESI ion source devices as claimed any one in claims 1 to 3, it is characterised in that also including fixed cover;
The fixed cover is installed on the atomizer, and the fixed cover is fixedly connected with the housing, is set in the fixed cover There is gas passage to be supplied for connection source of the gas and to the sheath gas passage.
5. ESI ion source devices as claimed in claim 4, it is characterised in that position adjustments rotation is additionally provided with the fixed cover Button, the position adjustments knob is used to adjust the position of the metal capillary.
6. ESI ion source devices as claimed in claim 5, it is characterised in that the position adjustments knob has 2 groups, wherein The group position adjustments knob is used to adjust the upper-lower position of the metal capillary, and position adjustments knob is used for described in another group Adjust the right position of the metal capillary.
7. ESI ion source devices as claimed in claim 1, it is characterised in that the housing is provided with observation window;The ion The bottom of source chamber room is provided with outlet.
8. a kind of mass spectrograph, it is characterised in that including any one of spectrometer body, connecting plate and claim 1 to 7 ESI ion source devices;
The spectrometer body includes mass spectrometer, and the mass spectrometer has ion sampling end, the ion sampling end Through hole through the connecting plate is stretched in the ion source chamber room, the connecting plate respectively with the spectrometer body and institute Housing is stated to be fixedly connected.
9. mass spectrograph as claimed in claim 8, it is characterised in that also including sealing ring, the sealing ring is arranged the ion Using on end for sealing the ion source chamber.
10. a kind of liquid chromatography mass combined instrument, it is characterised in that including the matter described in liquid chromatograph and claim 8 or 9 Spectrometer, the outlet of the liquid chromatograph is connected with the inlet of the metal capillary.
CN201621229362.9U 2016-11-15 2016-11-15 ESI ion source devices, mass spectrograph and liquid chromatography mass combined instrument Active CN206225322U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109979797A (en) * 2019-04-29 2019-07-05 昆山禾信质谱技术有限公司 One kind being used for mass spectrometric ion source device and its application method
CN110085506A (en) * 2018-01-26 2019-08-02 广州禾信仪器股份有限公司 Sample introduction assembly, open type ion source system and mass spectrometer
CN111480074A (en) * 2017-10-13 2020-07-31 阿基尔·卡皮耶洛 Chemical analyzer combining electron ionization mass spectrometry with liquid chromatography
CN111920979A (en) * 2020-09-07 2020-11-13 东华理工大学 Closed type ion source device that disappears

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111480074A (en) * 2017-10-13 2020-07-31 阿基尔·卡皮耶洛 Chemical analyzer combining electron ionization mass spectrometry with liquid chromatography
CN111480074B (en) * 2017-10-13 2022-12-27 阿基尔·卡皮耶洛 Chemical analyzer combining electron ionization mass spectrometry with liquid chromatography
CN110085506A (en) * 2018-01-26 2019-08-02 广州禾信仪器股份有限公司 Sample introduction assembly, open type ion source system and mass spectrometer
CN109979797A (en) * 2019-04-29 2019-07-05 昆山禾信质谱技术有限公司 One kind being used for mass spectrometric ion source device and its application method
CN109979797B (en) * 2019-04-29 2024-04-19 昆山禾信质谱技术有限公司 Ion source device for mass spectrometer and application method thereof
CN111920979A (en) * 2020-09-07 2020-11-13 东华理工大学 Closed type ion source device that disappears

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Address after: 510535 No. 16, Xinrui Road, Huangpu District, Guangzhou, Guangdong

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