CN204927235U - Sampling interface device for ionization source, mass spectrometer and liquid chromatography-mass spectrometer - Google Patents
Sampling interface device for ionization source, mass spectrometer and liquid chromatography-mass spectrometer Download PDFInfo
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- CN204927235U CN204927235U CN201520487795.3U CN201520487795U CN204927235U CN 204927235 U CN204927235 U CN 204927235U CN 201520487795 U CN201520487795 U CN 201520487795U CN 204927235 U CN204927235 U CN 204927235U
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Abstract
本实用新型提供一种电离源用进样接口装置、质谱仪和液相色谱质谱联用仪；电离源用进样接口装置包括液相毛细管，其具有液相进口；能够将液相毛细管的液相出口的液态样品转化为喷雾输送到离子源的出口与质谱分析器的离子采样口之间的电离区的气液喷管，其外套于液相毛细管并与液相毛细管形成气液通道并设置有鞘气进口和鞘液进口；用于向气液通道内输送预设气压的鞘气的鞘气管路，其与鞘气进口连通；用于向气液通道内输送鞘液的鞘液管路，其与鞘液进口连通；用于对从气液喷管的喷出口喷出的喷雾进行加热的加热件，其位于气液喷管的喷出口靠近电离区的一侧。本实用新型能降低无机盐及弱极性有机溶剂对质谱仪电离的影响，扩大了液质联用的应用范围。
The utility model provides a sampling interface device for an ionization source, a mass spectrometer and a liquid chromatography-mass spectrometer; the sampling interface device for an ionization source includes a liquid phase capillary, which has a liquid phase inlet; The liquid sample at the phase outlet is converted into a gas-liquid spray pipe that is transported to the ionization area between the outlet of the ion source and the ion sampling port of the mass spectrometer. There are sheath gas inlet and sheath liquid inlet; the sheath gas pipeline for delivering preset pressure sheath gas to the gas-liquid channel, which communicates with the sheath gas inlet; the sheath fluid pipeline for delivering sheath fluid to the gas-liquid channel , which communicates with the sheath liquid inlet; a heating element for heating the spray sprayed from the outlet of the gas-liquid nozzle, which is located on the side of the outlet of the gas-liquid nozzle close to the ionization region. The utility model can reduce the influence of inorganic salts and weak polar organic solvents on the ionization of mass spectrometers, and expands the application range of liquid mass spectrometry.
Description
Technical field
The utility model relates to detection analysis technical field, more particularly, relate to a kind of ionization source sample introduction interface arrangement, the utility model also relate to a kind of there is above-mentioned ionization source sample introduction interface arrangement mass spectrometer and one there is above-mentioned mass spectrometric liquid chromatography mass combined instrument.
Background technology
Mass-spectrometric technique by physics and chemistry means, target molecule is ionized, and utilizes electromagnetic field charged molecule to be distinguished the technology detected according to mass-to-charge ratio.This technology has the features such as fast, the highly sensitive and specificity of analysis speed is strong, is thus widely used at chemistry and the field such as chemical industry, biology and life science, medical science, pharmacy, material science, environmental protection science.Liquid-phase chromatographic analysis technology, comprise Capillary Electrophoresis, it is a kind of separation method of comparative maturity, have that separative efficiency is high, highly sensitive, quick, wide accommodation, the feature such as reproducible and easy to operate, be thus widely used in the clinical diagnosis of medical science, the quality control of medicine, the field such as drug metabolite analysis and pharmacokinetic.In recent years, high performance liquid chromatography and mass spectrographic successful coupling, achieve the strong separating power of liquid chromatogram and the combination of mass spectrographic high sensitivity and strong distinguishing ability, directly can carry out a point analysis of variance to the sample of complicated component.
The liquid sample that liquid chromatogram in capillary is separated is ionized and imports to mass ions transmission channel and detect by electron spray ionisation source (ESI) by existing LC-ESI/MS (liquid chromatograph-mass spectrometer).But, when containing fixedness inorganic salts (as inorganic buffer salt or hydrochloride etc.) in liquid sample, salt can be piled up at shower nozzle place, destroy the integrality of spraying, also can block mass ions transmission channel, further, the inhibitory action such as ionization and matrix effect of also competing of the low pole organic reagent in salt and liquid sample cause target molecule effectively to ionize.Therefore, the range of application of LC-MS is limited.
In sum, how reducing the impact that inorganic salts and weakly polar organic solvent ionize mass spectrometer, to expand the range of application of LC-MS, is current those skilled in the art technical problems urgently to be resolved hurrily.
Utility model content
In view of this, the purpose of this utility model is to provide a kind of ionization source sample introduction interface arrangement, to reduce the impact that inorganic salts and weakly polar organic solvent ionize mass spectrometer, thus expands the range of application of LC-MS.
Another object of the present utility model be to provide a kind of there is above-mentioned ionization source sample introduction interface arrangement mass spectrometer and one there is above-mentioned mass spectrometric liquid chromatography mass combined instrument.
In order to achieve the above object, the utility model provides following technical scheme:
A kind of ionization source sample introduction interface arrangement, comprising:
Liquid phase capillary, described liquid phase capillary has the fluid inlet entered for liquid sample;
The liquid sample of the liquid-phase outlet of described liquid phase capillary can be converted into the gas-liquid jet pipe of the ionized region between the ion thief hatch being transported to ionogenic outlet and mass spectrometer of spraying, described gas-liquid jet pipe is coated at described liquid phase capillary and also and between described liquid phase capillary forms gas-liquid channel, described gas-liquid jet pipe is provided with the import of sheath gas and sheath fluid import;
For carrying the sheath air pipe of the sheath gas of preset pressure in described gas-liquid channel, described sheath air pipe and described sheath gas inlet communication;
For carrying the sheath liquid pipeline of sheath fluid in described gas-liquid channel, described sheath liquid pipeline and described sheath fluid inlet communication;
For the heating member that the spraying sprayed the ejiction opening from described gas-liquid jet pipe is heated, described heating member is positioned at the side of ejiction opening near described ionized region of described gas-liquid jet pipe.
Preferably, in above-mentioned ionization source sample introduction interface arrangement, the liquid-phase outlet of described liquid phase capillary protrudes from the ejiction opening of described gas-liquid jet pipe.
Preferably, in above-mentioned ionization source sample introduction interface arrangement, the port of export of described gas-liquid jet pipe is from the one end away from described ionized region to the tapered at one end near described ionized region, and the ejiction opening diameter of described gas-liquid jet pipe is 0.8mm-1.2mm;
The liquid-phase outlet of described liquid phase capillary is 0.3mm-0.5mm apart from the distance of the ejiction opening of described gas-liquid jet pipe.
Preferably, in above-mentioned ionization source sample introduction interface arrangement, the port of export of described gas-liquid jet pipe is tapered injection outlet, and described tapered injection outlet removably connects with the straight length of described gas-liquid jet pipe.
Preferably, in above-mentioned ionization source sample introduction interface arrangement, described heating member is the cylindrical sleeves being coated at described gas-liquid jet pipe, and described cylindrical sleeves has heating part near the side of described ionized region;
Described ionization source sample introduction interface arrangement also comprises base, described cylindrical sleeves to be arranged on described base and to be fixedly connected with described gas-liquid jet pipe by bolt, described cylindrical sleeves is provided with the tapped through hole passed for described bolt, outer wall and the described bolt of described gas-liquid jet pipe offset, and described gas-liquid jet pipe outer wall have many fixing marking lines axially arranged along it.
Preferably, in above-mentioned ionization source sample introduction interface arrangement, described cylindrical sleeves is by the first micrometer, second micrometer and the 3rd micrometer are arranged on described base, the micrometric screw of described first micrometer is along X to setting, the micrometric screw of described second micrometer is arranged along Y-direction, the micrometric screw of described 3rd micrometer is arranged along Z-direction, the framework of described second micrometer is fixed on the micrometric screw of described first micrometer, the framework of described 3rd micrometer is fixed on the micrometric screw of described second micrometer, described cylindrical sleeves is fixedly installed on the micrometric screw of described 3rd micrometer, wherein, X to, Y-direction, Z-direction be vertical between two.
Preferably, in above-mentioned ionization source sample introduction interface arrangement, described cylindrical sleeves is also arranged with ceramic cylinder outward, and described ceramic cylinder is connected with the threaded one end of described cylindrical sleeves away from described ionized region away from one end of described ionized region.
Preferably, in above-mentioned ionization source sample introduction interface arrangement, also comprise:
Control the operating voltage of described heating member and the control cabinet of temperature;
Regulate described sheath air pipe to be transported to the diaphragm valve of the sheath atmospheric pressure in described gas-liquid jet pipe, described diaphragm valve is arranged on described sheath air pipe.
As can be seen from above-mentioned technical scheme, the ionization source sample introduction interface arrangement that the utility model provides comprises liquid phase capillary, gas-liquid jet pipe, sheath air pipe, sheath liquid pipeline and heating member; Wherein, liquid phase capillary has the fluid inlet entered for liquid sample; The liquid sample of the liquid-phase outlet of liquid phase capillary can be converted into the ionized region between the ion thief hatch being transported to ionogenic outlet and mass spectrometer of spraying by gas-liquid jet pipe, gas-liquid jet pipe is coated at liquid phase capillary and also and between liquid phase capillary forms gas-liquid channel, gas-liquid jet pipe is provided with the import of sheath gas and sheath fluid import; Sheath air pipe is used for the sheath gas carrying preset pressure in gas-liquid channel, sheath air pipe and sheath gas inlet communication; Sheath liquid pipeline is used in gas-liquid channel, carrying sheath fluid, sheath liquid pipeline and sheath fluid inlet communication; Heating member is used for heating the spraying that the ejiction opening from gas-liquid jet pipe sprays, and heating member is positioned at the side of ejiction opening near ionized region of gas-liquid jet pipe.
During application, first liquid sample is imported liquid phase capillary from fluid inlet; Pass through sheath air pipe to delivery sheath gas in gas-liquid channel simultaneously, in gas-liquid channel, sheath fluid is carried by sheath liquid pipeline, thus make the gas-liquid mixture fluid being full of preset pressure (generally at 5kPa to 10kPa) in gas-liquid channel, the liquid sample that the liquid-phase outlet of liquid phase capillary flows out can be driven to be converted into spraying together in the process that gas-liquid mixture fluid flows out to ejiction opening; Then heating member heats whole spraying, the gas-liquid mixture launched from ejiction opening is fully heated, and then determinand molecule is gasified, inorganic salt molecule bunch is polymerized to solid-state crystallite, thus can determinand molecule effectively in separation of liquid sample and inorganic salts, as phosphate, carbonate, borate, hydrochloride etc.; By determinand molecular jet in the ionized region between ionogenic outlet and the ion thief hatch of mass spectrometer, the solvent volatilized in this process such as the protonated solvent such as water, methyl alcohol can improve the ionizing efficiency of ionization source, and weakly polar organic solvent is difficult to be combined with proton and generates quasi-molecular ion, compete ionizing hardly with determinand.
In summary, ionization source sample introduction interface arrangement of the present utility model can reduce the impact that inorganic salts and weakly polar organic solvent ionize mass spectrometer, thus expands the range of application of LC-MS.
The utility model additionally provides a kind of mass spectrometer, comprise mass ion source and mass spectrometer, described mass ion source is DART ionization source, described mass spectrometer also comprises the sample introduction interface arrangement for liquid sample being transported to described DART ionization source, described sample introduction interface arrangement is any one ionization source sample introduction interface arrangement above-mentioned, because above-mentioned ionization source sample introduction interface arrangement has above-mentioned effect, the mass spectrometer with above-mentioned ionization source sample introduction interface arrangement has same effect, therefore repeats no more herein.
The utility model additionally provides a kind of liquid chromatography mass combined instrument, comprise chromatograph and export with described chromatographic liquid sample the mass spectrometer be connected, described mass spectrometer is any one mass spectrometer above-mentioned, because above-mentioned mass spectrometer has above-mentioned effect, there is above-mentioned mass spectrometric liquid chromatography mass combined instrument there is same effect, therefore repeat no more herein.
Accompanying drawing explanation
In order to be illustrated more clearly in the utility model embodiment or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is embodiments more of the present utility model, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the partial structurtes schematic diagram of the ionization source sample introduction interface arrangement that the utility model embodiment provides;
Fig. 2 is another partial structurtes schematic diagram of the ionization source sample introduction interface arrangement that the utility model embodiment provides.
Embodiment
The utility model embodiment provides a kind of ionization source sample introduction interface arrangement, can reduce the impact that inorganic salts and weakly polar organic solvent ionize mass spectrometer, thus expands the range of application of LC-MS.
For making the object of the utility model embodiment, technical scheme and advantage clearly, below in conjunction with the accompanying drawing in the utility model embodiment, technical scheme in the utility model embodiment is clearly and completely described, obviously, described embodiment is the utility model part embodiment, instead of whole embodiments.Based on the embodiment in the utility model, those of ordinary skill in the art are not making the every other embodiment obtained under creative work prerequisite, all belong to the scope of the utility model protection.
Please refer to accompanying drawing 1-2, the ionization source sample introduction interface arrangement that the utility model embodiment provides comprises liquid phase capillary 1, gas-liquid jet pipe 2, sheath air pipe 4, sheath liquid pipeline 5 and heating member; Wherein, liquid phase capillary 1 has the fluid inlet entered for liquid sample; The liquid sample of the liquid-phase outlet of liquid phase capillary 1 can be converted into the ionized region between the ion thief hatch being transported to ionogenic outlet and mass spectrometer of spraying by gas-liquid jet pipe 2, gas-liquid jet pipe 2 is coated at liquid phase capillary 1 and also and between liquid phase capillary 1 forms gas-liquid channel, gas-liquid jet pipe 2 is provided with the import of sheath gas and sheath fluid import; Sheath air pipe 4 for carrying the sheath gas of preset pressure in gas-liquid channel, sheath air pipe 4 and sheath gas inlet communication; Sheath liquid pipeline 5 for carrying sheath fluid in gas-liquid channel, sheath liquid pipeline 5 and sheath fluid inlet communication; Heating member is used for heating the spraying that the ejiction opening from gas-liquid jet pipe 2 sprays, and heating member is positioned at the side of ejiction opening near ionized region of gas-liquid jet pipe 2.
It should be noted that, above-mentioned sheath air pipe 4 is transported to the axial flow of the sheath gas in gas-liquid channel along liquid phase capillary 1, drives the liquid sample uniformly continous spraying of flowing out from liquid phase capillary 1 together with sheath fluid.Concrete, in order to reduce gravity effect, gas-liquid jet pipe 2 is vertically arranged, and the ion thief hatch of ionogenic outlet and mass spectrometer is positioned on same level line, forms ionized region between the two, and gas-liquid jet pipe 2 is arranged at above ionized region; Heating member is positioned at the side of ejiction opening near ionized region of gas-liquid jet pipe 2, and namely heating member is positioned at immediately below the ejiction opening of gas-liquid jet pipe 2, heats whole spraying, has good signal effect.
Above-mentioned liquid sample can be fluid sample direct injected and the liquid sample through chromatographic isolation.
During application, first liquid sample is imported liquid phase capillary 1 from fluid inlet; Pass through sheath air pipe 4 to delivery sheath gas in gas-liquid channel simultaneously, in gas-liquid channel, sheath fluid is carried by sheath liquid pipeline 5, thus make the gas-liquid mixture fluid being full of preset pressure (generally at 5kPa to 10kPa) in gas-liquid channel, the liquid sample that the liquid-phase outlet of liquid phase capillary 1 flows out can be driven to be converted into spraying together in the process that gas-liquid mixture fluid flows out to ejiction opening; Then heating member heats whole spraying, the gas-liquid mixture launched from ejiction opening is fully heated, and then determinand molecule is gasified, inorganic salt molecule bunch is polymerized to solid-state crystallite, thus can determinand molecule effectively in separation of liquid sample and inorganic salts, as phosphate, carbonate, borate, hydrochloride etc.; By determinand molecular jet in the ionized region between ionogenic outlet and the ion thief hatch of mass spectrometer, the solvent volatilized in this process such as the protonated solvent such as water, methyl alcohol can improve the ionizing efficiency of ionization source, and weakly polar organic solvent is difficult to be combined with proton and generates quasi-molecular ion, compete ionizing hardly with determinand.
In summary, ionization source sample introduction interface arrangement of the present utility model can reduce the impact that inorganic salts and weakly polar organic solvent ionize mass spectrometer, thus expands the range of application of LC-MS.
In specific embodiment, the determinand molecular jet that gasification separation goes out by ionization source sample introduction interface arrangement of the present utility model is to the DART (abbreviation of DirectAnalysisinRealTime, Direct Analysis in Real Time) in ionized region between the outlet of ionization source and the ion thief hatch of mass spectrometer, by introducing in mass spectrographic mass spectrometer after DART ionization, be applicable to the Mass Spectrometer Method of fluid sample direct injected and the liquid sample through chromatographic isolation.
In order to reach good spray effect, in the ionization source sample introduction interface arrangement that above-described embodiment provides, the liquid-phase outlet of liquid phase capillary 1 protrudes from the ejiction opening of gas-liquid jet pipe 2.Now, namely near the side of ionized region outside the ejiction opening that the liquid-phase outlet of liquid phase capillary 1 is positioned at gas-liquid jet pipe 2, be convenient to drive liquid sample to form spraying.Certainly, the liquid-phase outlet of above-mentioned liquid phase capillary 1 also can be arranged at inside the ejiction opening of gas-liquid jet pipe 2.
Further, as shown in Figure 1-2, the port of export of gas-liquid jet pipe 2 is from the one end away from ionization source to the tapered at one end near ionization source, and the ejiction opening diameter of gas-liquid jet pipe 2 is 0.8mm-1.2mm, is preferably 1mm; The liquid-phase outlet of liquid phase capillary 1, apart from the distance 0.3mm-0.5mm of the ejiction opening of gas-liquid jet pipe 2, is preferably 0.5mm.So, gas-liquid jet pipe 2 has less ejiction opening, accelerate the flow velocity of sheath fluid sheath gas fluid-mixing at ejiction opening place, coordinate the sheath gas in gas-liquid channel and sheath fluid that the liquid sample of liquid-phase outlet can be driven to obtain the blended atomize of good gas-liquid, thus make, between determinand molecule and inorganic salts, there is good separating effect.The above-mentioned ejiction opening reduced can also swing by limits liquid phase capillary 1 to a certain extent simultaneously.Be understandable that, above-mentioned gas-liquid jet pipe 2 can be also straight tube shape, as long as can realize driving liquid sample to reach the shape of atomize.
In order to optimize technique scheme, the port of export of gas-liquid jet pipe 2 is tapered injection outlet, and tapered injection outlet removably connects with the straight length of gas-liquid jet pipe 2.Now, the surface of gas-liquid jet pipe 2 is taper seat, is convenient to processing.Concrete, this tapered injection outlet utilization is threaded and achieves detachably, only can change ejiction opening, saved cost, be convenient to dismounting simultaneously when tapered injection outlet wearing and tearing are more serious.The port of export of this gas-liquid jet pipe 2 also can be the tapered shape of multiple plane formation or Surface forming
In order to make spraying be heated evenly, preferably, heating member is the cylindrical sleeves 3 being coated at gas-liquid jet pipe 2, and cylindrical sleeves 3 has heating part 31 near the side of ionized region; In order to reduce gravity effect, gas-liquid jet pipe 2 is vertically arranged, the outlet of DART and the ion thief hatch of mass spectrographic mass spectrometer are positioned on same level line, form ionized region between the two, gas-liquid jet pipe 2 is arranged at above ionized region, and the top of cylindrical sleeves 3 is set in outside gas-liquid jet pipe 2, and bottom is provided with heating part 31, the below being positioned at gas-liquid jet pipe 2 is heated whole spraying, and signal effect is better.Interchangeable, above-mentioned heating member can also for the multiple heating plates circumferentially arranged.
For the ease of installing, ionization source sample introduction interface arrangement also comprises base (not shown), cylindrical sleeves 3 to be arranged on base and to be fixedly connected with gas-liquid jet pipe 2 by bolt, cylindrical sleeves 3 is provided with the tapped through hole passed for bolt, outer wall and the bolt of gas-liquid jet pipe 2 offset, and gas-liquid jet pipe 2 outer wall have many fixing marking lines axially arranged along it.The utility model passes the tapped through hole on cylindrical sleeves 3 by making bolt and offsets with the outer wall of gas-liquid jet pipe 2, utilizes bolt to oppress gas-liquid jet pipe 2 outer wall and produces trickle Metal Deformation banding cylindrical sleeves 3 and gas-liquid jet pipe 2.According to the difference detecting liquid sample, the utility model is also by the height and position of adjustment gas-liquid jet pipe 2, make bolt-locking in the position of the corresponding fixed table timberline of gas-liquid jet pipe 2, thus by changing the height of gas-liquid jet pipe 2, relative position between the ejiction opening achieving heating part 31 and gas-liquid jet pipe 2 is adjustable, thus make liquid sample reach good released state by adjustment, improve ionization effect.Certainly, cylindrical sleeves 3 and gas-liquid jet pipe 2 can also be achieved a fixed connection by other structures, as the joint pin etc. be weldingly connected with both respectively.
In order to optimize technique scheme further, above-mentioned cylindrical sleeves 3 is arranged on base by the first micrometer, the second micrometer and the 3rd micrometer, the micrometric screw of the first micrometer is along X to setting, the micrometric screw of the second micrometer is arranged along Y-direction, the micrometric screw of the 3rd micrometer is arranged along Z-direction, the framework of the second micrometer is fixed on the micrometric screw of the first micrometer, the framework of the 3rd micrometer is fixed on the micrometric screw of the second micrometer, and cylindrical sleeves 3 is fixedly installed on the micrometric screw of the 3rd micrometer; Wherein, X to, Y-direction, Z-direction be vertical between two.The utility model makes cylindrical sleeves 3 can be three-dimensional adjustable relative to base by three micrometers, thus by regulating the ejiction opening of gas-liquid jet pipe 2 relative to the three-dimensional position of DART and mass spectrographic mass spectrometer, stable detection signal can be obtained when analyzing different buffer salt system and different organic solvents system.
This ionization source sample introduction interface arrangement can be integrated and use with efficient/Ultra Performance Liquid Chromatography/Capillary Electrophoresis-DART ionization source-mass spectrometer, carry out open type atmospheric pressure ionization and introduce mass spectrum carrying out analyzing and testing to through the sample of liquid phase separation or the liquid sample of direct injected, this device improves the requirement of LC-MS to liquid phase buffer salt, and strengthens signal strength signal intensity and the stability of DART detection.
Certainly, the utility model can also realize cylindrical sleeves 3 by other devices can be three-dimensional adjustable relative to base, if the X that forms by line slide rail, ball-screw and servomotor is to, the motion of Y-direction, Z-direction.
Cylindrical sleeves 3 is outer is also arranged with ceramic cylinder (not shown), and ceramic cylinder is connected with the threaded one end of cylindrical sleeves 3 away from ionized region away from one end of ionized region.Above-mentioned ceramic cylinder can be incubated heating part 31, realizes thermal-arrest and restriction air-flow, makes liquid sample reach better separating effect.
Preferably, ionization source sample introduction interface arrangement also comprises the control operating voltage of heating member and the control cabinet of temperature; Regulate sheath air pipe 4 to be transported to the diaphragm valve of the sheath atmospheric pressure in gas-liquid jet pipe 2, diaphragm valve is arranged on sheath air pipe 4.In specific works process, heating member operating voltage is 24V, by the temp controlled meter control temperature of control cabinet.The pressure of sheath air-flow can be regulated by diaphragm valve as required.Can also by controlling the stable detection signal of the gain of parameter such as heating-up temperature and sheath gas velocity when the different buffer salt system of this device analysis and different organic solvents system.
For the ease of assembling, above-mentioned liquid phase capillary 1 is fixed on gas-liquid jet pipe 2 away from one end of ionization source and top by graphite gasket, graphite gasket is sheathed and be sealed between liquid phase capillary 1 and gas-liquid jet pipe 2, and the import of sheath gas and sheath fluid import are positioned at the side of graphite gasket near ionization source.Now as required, by regulating the relative position of graphite gasket and liquid phase capillary 1, the relative position of the liquid-phase outlet of liquid phase capillary 1 and the ejiction opening of gas-liquid jet pipe 2 can be regulated.
Further, the internal diameter of liquid phase capillary 1 is 75 μm-150 μm.Liquid phase capillary 1 is the quartz capillary that metal capillary or top layer have polyimide coating, thus makes liquid phase capillary 1 bent, is convenient to adjust its position, reduces the damage because of bending generation in the course of work simultaneously.Above-mentioned polyimides, has good resistant of high or low temperature, electric insulating quality, caking property, radiation resistance, resistance to medium, and chemical stability and anti-flammability improve the useful life of liquid phase capillary 1.
The utility model also arranges waste collecting device in the below of ionized region, is convenient to the waste liquid collecting ejection.
The utility model embodiment still provides a kind of mass spectrometer, comprise mass ion source and mass spectrometer, mass ion source is DART ionization source, mass spectrometer also comprises the sample introduction interface arrangement for liquid sample being transported to DART ionization source, the ionization source sample introduction interface arrangement that sample introduction interface arrangement provides for above-mentioned any one embodiment, the impact that inorganic salts and weakly polar organic solvent ionize mass spectrometer can be reduced, thus expand the range of application of LC-MS; Its advantage is brought by ionization source sample introduction interface arrangement, and concrete please refer to part relevant in above-described embodiment, just repeats no more at this.
In an embodiment of concrete practice:
Ionization source sample introduction interface arrangement optimum configurations: heating-up temperature is 250 DEG C, sheath gas air pressure is 5kPa, DART temperature is 350 DEG C, and DART and mass spectrometer distance are 10mm, and ejiction opening is positioned at distance mass spectrometer 7mm above DART and mass spectrometer line.
Liquid sample to be measured is reserpine, and concentration 5 μ g/mL, water-soluble/acetonitrile is that in the solution of 1:1, solution system contains 137mMNaCl, 2.7mMKCl, 10mMNa
2hPO
4, 2mMKH
2pO
4.
This sample enters this device by peristaltic pump with the flow velocity of 200 μ L/min, eliminates the interference of inorganic salinity, obtains good ionization effect.
In another embodiment of concrete practice:
Ionization source sample introduction interface arrangement optimum configurations: device heating-up temperature is 260 DEG C, sheath gas air pressure is 10kPa, DART temperature is 350 DEG C, and DART and mass spectrometer distance are 15mm, and ejiction opening is positioned at distance mass spectrum 10mm above DART and mass spectrometer line.
Testing sample is seven kinds of benzodiazepines such as Lorazepam, Clonazepam, diazepam, Oxazepam, nitrazepam, chlordiazepoxide and midazolam maleate, after dissolving in methyl alcohol, be diluted to concentration with phosphoric acid-potassium dihydrogen phosphate that pH is 2.5 and be respectively 30-150 μ g/mL.
Biased sample passes through liquid chromatogram, be separated in the mode of gradient elution, and introduce this device, after DART ionization, the separating degree of the LC-MS spectrogram that obtains and simple liquid phase separation does not have notable difference, seven kinds of materials all can good electrical from and be not subject to phosphatic impact.
The DART ionization source that the utility model adopts has good tolerance to inorganic salts and aprotic solvents, weak polar solvent.DART (Direct Analysis in Real Time technology) ionization source is a kind of novel open type atmospheric pressure ionization techniques.DART technology develops based on Atmosphere Pressure Chemical Ionization (APCI) (APCI) principle, and carrying out ionization by the mode of this molecule-ionic reaction can ionize target molecule under sample is containing higher salinity and stronger matrix effect situation.The water that its main ionization process mainly comprises in excitation state gas (as nitrogen, helium or argon gas) atom and the surrounding air that electric discharge produces reacts, by formation water cluster from
Son and then carry out ionizing with the mode that sample molecule reacts the quasi-molecular ion generating determinand and in excitation state gas atom and gas phase, determinand molecule directly reacts the mode generating molecular ion and carries out ionization and Penning ionization (Penningionization) two kinds of principles.
The solvent volatilized in this process such as the protonated solvent such as water, methyl alcohol can improve the ionizing efficiency of DART.After DART ionization, the separating degree of the LC-MS spectrogram that obtains and simple liquid phase separation does not have notable difference, seven kinds of materials all can good electrical from and be not subject to phosphatic impact.
The utility model embodiment still provides a kind of liquid chromatography mass combined instrument, comprise chromatograph and export with chromatographic liquid sample the mass spectrometer be connected, mass spectrometer is above-mentioned mass spectrometer, because above-mentioned mass spectrometer has above-mentioned effect, there is above-mentioned mass spectrometric liquid chromatography mass combined instrument there is same effect, therefore repeat no more herein.
The utility model realizes liquid chromatogram and DART-MS combination analysis.And by the kind of the position of optimizing liquid phase stream effluent and mass spectrum entrance, secondary solvent, ionize relevant parameters, realize the qualitative and quantitative analysis to heterogeneity compound, and can set up according to result of study the LC-DART-MS analytical method comprising and be applicable to traditional Chinese medicine complex system and biological sample.The utility model will expand the application of DART in association area greatly, and the requirement of LC-MS to liquid phase buffer salt is relaxed further.
In this specification, each embodiment adopts the mode of going forward one by one to describe, and what each embodiment stressed is the difference with other embodiments, between each embodiment identical similar portion mutually see.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the utility model.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein when not departing from spirit or scope of the present utility model, can realize in other embodiments.Therefore, the utility model can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. an ionization source sample introduction interface arrangement, is characterized in that, comprising:
Liquid phase capillary (1), described liquid phase capillary (1) has the fluid inlet entered for liquid sample;
The liquid sample of the liquid-phase outlet of described liquid phase capillary (1) can be converted into the gas-liquid jet pipe (2) of the ionized region between the ion thief hatch being transported to ionogenic outlet and mass spectrometer of spraying, described gas-liquid jet pipe (2) be coated at described liquid phase capillary (1) and and form gas-liquid channel between described liquid phase capillary (1), described gas-liquid jet pipe (2) is provided with the import of sheath gas and sheath fluid import;
For carrying the sheath air pipe (4) of the sheath gas of preset pressure in described gas-liquid channel, described sheath air pipe (4) and described sheath gas inlet communication;
For carrying the sheath liquid pipeline (5) of sheath fluid in described gas-liquid channel, described sheath liquid pipeline (5) and described sheath fluid inlet communication;
For the heating member that the spraying sprayed the ejiction opening from described gas-liquid jet pipe (2) is heated, described heating member is positioned at the side of ejiction opening near described ionized region of described gas-liquid jet pipe (2).
2. ionization source sample introduction interface arrangement as claimed in claim 1, it is characterized in that, the liquid-phase outlet of described liquid phase capillary (1) protrudes from the ejiction opening of described gas-liquid jet pipe (2).
3. ionization source sample introduction interface arrangement as claimed in claim 2, it is characterized in that, the port of export of described gas-liquid jet pipe (2) is from the one end away from described ionized region to the tapered at one end near described ionized region, and the ejiction opening diameter of described gas-liquid jet pipe (2) is 0.8mm-1.2mm;
The liquid-phase outlet of described liquid phase capillary (1) is 0.3mm-0.5mm apart from the distance of the ejiction opening of described gas-liquid jet pipe (2).
4. ionization source sample introduction interface arrangement as claimed in claim 3, is characterized in that, the port of export of described gas-liquid jet pipe (2) is tapered injection outlet, and described tapered injection outlet removably connects with the straight length of described gas-liquid jet pipe (2).
5. ionization source sample introduction interface arrangement as claimed in claim 1, it is characterized in that, described heating member is for being coated at the cylindrical sleeves (3) of described gas-liquid jet pipe (2), and described cylindrical sleeves (3) has heating part (31) near described ionogenic side;
Described ionization source sample introduction interface arrangement also comprises base, described cylindrical sleeves (3) to be arranged on described base and to be fixedly connected with described gas-liquid jet pipe (2) by bolt, described cylindrical sleeves (3) is provided with the tapped through hole passed for described bolt, outer wall and the described bolt of described gas-liquid jet pipe (2) offset, and described gas-liquid jet pipe (2) outer wall have many fixing marking lines axially arranged along it.
6. ionization source sample introduction interface arrangement as claimed in claim 5, it is characterized in that, described cylindrical sleeves (3) is by the first micrometer, second micrometer and the 3rd micrometer are arranged on described base, the micrometric screw of described first micrometer is along X to setting, the micrometric screw of described second micrometer is arranged along Y-direction, the micrometric screw of described 3rd micrometer is arranged along Z-direction, the framework of described second micrometer is fixed on the micrometric screw of described first micrometer, the framework of described 3rd micrometer is fixed on the micrometric screw of described second micrometer, described cylindrical sleeves (3) is fixedly installed on the micrometric screw of described 3rd micrometer, wherein, X to, Y-direction, Z-direction be vertical between two.
7. the sample introduction interface arrangement of the ionization source as described in claim 5 or 6, it is characterized in that, described cylindrical sleeves (3) is also arranged with ceramic cylinder outward, and described ceramic cylinder is connected with the threaded one end of described cylindrical sleeves (3) away from described ionized region away from one end of described ionized region.
8. ionization source sample introduction interface arrangement as claimed in claim 1, is characterized in that, also comprise:
Control the operating voltage of described heating member and the control cabinet of temperature;
Regulate described sheath air pipe (4) to be transported to the diaphragm valve of the sheath atmospheric pressure in described gas-liquid jet pipe (2), described diaphragm valve is arranged on described sheath air pipe (4).
9. a mass spectrometer, comprise mass ion source and mass spectrometer, it is characterized in that, described mass ion source is DART ionization source, described mass spectrometer also comprises the sample introduction interface arrangement for liquid sample being transported to described DART ionization source, and described sample introduction interface arrangement is the ionization source sample introduction interface arrangement as described in any one of claim 1-8.
10. a liquid chromatography mass combined instrument, comprise chromatograph and export with described chromatographic liquid sample the mass spectrometer be connected, it is characterized in that, described mass spectrometer is mass spectrometer as claimed in claim 9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201520487795.3U CN204927235U (en) | 2015-07-08 | 2015-07-08 | Sampling interface device for ionization source, mass spectrometer and liquid chromatography-mass spectrometer |
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| CN201520487795.3U CN204927235U (en) | 2015-07-08 | 2015-07-08 | Sampling interface device for ionization source, mass spectrometer and liquid chromatography-mass spectrometer |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104966657A (en) * | 2015-07-08 | 2015-10-07 | 中国科学院长春应用化学研究所 | Sample introduction interface device for ionization source, mass spectrometry and liquid phase gas chromatograph-mass spectrometer |
| CN108499499A (en) * | 2018-04-03 | 2018-09-07 | 同济大学 | A kind of miniature continuous flow-tube reactor of controllable temperature |
| CN110208039A (en) * | 2019-06-27 | 2019-09-06 | 山东安准智能科技有限公司 | A kind of sampler, quickly heating sampling system and rapid detection method |
| CN112326771A (en) * | 2020-11-06 | 2021-02-05 | 北京印刷学院 | An analytical electrospray ionization device |
| CN113189458A (en) * | 2021-04-28 | 2021-07-30 | 中国烟草总公司郑州烟草研究院 | Ultrasonic atomization corona discharge mass spectrum device for researching droplet interface reaction |
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2015
- 2015-07-08 CN CN201520487795.3U patent/CN204927235U/en not_active Withdrawn - After Issue
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104966657A (en) * | 2015-07-08 | 2015-10-07 | 中国科学院长春应用化学研究所 | Sample introduction interface device for ionization source, mass spectrometry and liquid phase gas chromatograph-mass spectrometer |
| CN108499499A (en) * | 2018-04-03 | 2018-09-07 | 同济大学 | A kind of miniature continuous flow-tube reactor of controllable temperature |
| CN108499499B (en) * | 2018-04-03 | 2020-11-27 | 同济大学 | A temperature-controllable micro-continuous flow tube reactor |
| CN110208039A (en) * | 2019-06-27 | 2019-09-06 | 山东安准智能科技有限公司 | A kind of sampler, quickly heating sampling system and rapid detection method |
| CN110208039B (en) * | 2019-06-27 | 2021-12-10 | 山东安准智能科技有限公司 | Sampler, rapid heating sample introduction system and rapid detection method |
| CN112326771A (en) * | 2020-11-06 | 2021-02-05 | 北京印刷学院 | An analytical electrospray ionization device |
| CN112326771B (en) * | 2020-11-06 | 2022-07-22 | 北京印刷学院 | Analytic electrospray ionization device |
| CN113189458A (en) * | 2021-04-28 | 2021-07-30 | 中国烟草总公司郑州烟草研究院 | Ultrasonic atomization corona discharge mass spectrum device for researching droplet interface reaction |
| CN113189458B (en) * | 2021-04-28 | 2024-04-30 | 中国烟草总公司郑州烟草研究院 | Ultrasonic atomization corona discharge mass spectrum device for researching liquid drop interface reaction |
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