CN202120862U - Normal pressure chemical extraction ionization source - Google Patents
Normal pressure chemical extraction ionization source Download PDFInfo
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- CN202120862U CN202120862U CN2011202368912U CN201120236891U CN202120862U CN 202120862 U CN202120862 U CN 202120862U CN 2011202368912 U CN2011202368912 U CN 2011202368912U CN 201120236891 U CN201120236891 U CN 201120236891U CN 202120862 U CN202120862 U CN 202120862U
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Abstract
The utility model relates to a normal pressure chemical extraction ionization source, equipped with an ionization pipe and a sample pipe. The ionization pipe and the sample pipe are aslant arranged within an included angle and a distance, and the ports of the ionization pipe and the sample pipe point an ionization area jointly. The sample pipe comprises a sample inlet pipe and a sample carrying gas pipe, a gas or liquid sample is guided in the sample inlet pipe or the sample inlet pipe is communicated with a sample eduction pipe of a neutral desorbing device. The method of utilizing the normal pressure chemical extraction ionization source of the utility model comprises the steps of using a sample flow educed from the sample pipe and an ion flow educed from the ionization pipe to impact with each other to occur the extraction ionization, and then carrying out a mass spectrometry. The normal pressure chemical extraction ionization source is especially suitable for the real-time rapid analysis of complicated samples, such as biological sample, food, drugs, environmental sample, etc.
Description
Technical field
The utility model belongs to the mass spectral analysis field, relates to mass spectrometric normal pressure mass spectrum ionization source, is a kind of normal pressure chemical extraction ionization source specifically.
Background technology
Mass spectrography is one of most important method of analysis field; Along with development of science and technology; Mass spectrum not only occupies critical role in the conventional chemical analysis, and become life science gradually, Homeland Security, food security, clinical medicine detect and one of the main method of popular domain such as space technology.Thereupon, the used ionization source of mass spectrum has also obtained development at full speed, and various novel ion sources, new technology are also constantly emerged in large numbers.The mass spectrometric analysis method of original position, real-time, online, non-destruction, high flux, low-loss is one of target of pursuing of people always, is an important trend of mass-spectrometric technique development.
Mass spectrometer itself generally partly is made up of sample drawing-in system, ion source, ion-optic system, mass analyzer, detector, acquisition and control system, vacuum system etc.Mass-spectrometry and mass spectrometer developing history show that new ionogenic development and exploitation have the meaning of particular importance.The mass spectrum scholar generally believes no matter be to organic mass spectrometry or inorganic mass spectrum, the heart of mass spectrometer all is ionization sources.U.S. scientist John Fen En (John B.Fenn) exactly because etc. obtained Nobel chemistry Prize in 2002 having made major contribution aspect development electron spray ionisation (ESI) this soft ionization source.Yet the mass spectral ionization source of development and exploitation can carry out ionization after all requiring sample is converted into specific form in last 100 years.Therefore, in these conventional ionization sources,, sample must carry out The pretreatment before being measured.In fact, to obtaining data, the needed time of mass spectrography measuring process itself is no more than the several seconds from sample introduction, but the time of sample pretreatment then possibly reach several hours even a couple of days.In some important use occasions; On-the-spot on-line determination like the pharmaceuticals industry Chinese medicine tablet; The monitoring of trace explosive on the luggage, the quality of food is identified, the commodity inspection in the foreign trade; Live body pharmacokinetics research etc. are all hoped and can need not carried out nondestructive fast measuring to sample under the situation of sample pretreatment.
Get into 21 century, people have carried out bold exploration for the mass spectrum rapid analysis of complicated substrate sample, have obtained important progress.2004; Professor Cooks of Purdue university waits and on Science, has delivered first piece of article about electron spray desorption ionization (DESI); Need not carry out under the situation of sample pretreatment; Successfully obtained the mass spectrum of trace materials on the different surfaces, for realize need not sample pretreatment mass spectrometric analysis method opened a window.The DESI technology has caused ardent repercussion immediately in the world, and many in the world groups have begun the research of this respect immediately.After 1 year; Chinese scholar exploitation with DESI similarly in addition a kind of novel ionization source (EESI) technology be published on the Britain Chem.Commun. magazine, have important application at the complex samples such as analysis monitoring, environmental monitoring and analysis of biological sample monitoring and metabolic analysis research, food and medicine.Research shows that DESI and EESI are the important tool of analyzing nonpolar molecule, in a lot of occasions or even preferred option.Consider the deficiency that DESI and EESI detect and analyze at nonpolar molecule; Utility model people in 2005 etc. have developed surface desorption chemical ionization source (DAPCI); Can directly survey the nonpolar molecule in the complex sample in the surface need not sample pretreatment, this technology ZL200710307112.1 that patented.This technology has bright development prospect for the quick mass spectral analysis aspect of complicated substrate material in the surface; Yet in using; Utility model people finds that also also there is shortcoming in the DAPCI device; The analytic sample continuously owing to adopt surperficial sample introduction that sample will be reduced in desorption process gradually, and can not desorb nonpolar molecule and the big molecule of ionized biological.
The utility model content
The technical problem that the utility model solves is; Solve the problem that the surface chemistry ionization source can not the continuous sample introduction analysis and can not the desorb large biological molecule; And extract the problem that ionization source can not directly be analyzed nonpolar molecule, provide a kind of assembly difficulty low, low cost of manufacture; Ionization Efficiency is high, highly sensitive normal pressure chemical extraction ionization source.
The normal pressure chemical extraction ionization source of the utility model; Be provided with ionization tube and sample cell; Ionization tube and sample cell point to ionized space jointly with an angle and the oblique placement of a spacing and port; It is characterized in that: sample cell comprises a sample inlet tube and sample carrier gas pipe, imports gas or fluid sample in the sample inlet tube or connects the sample delivery line of a neutral desorption apparatus.
Wherein, said ionization tube comprises that an ionic tube is connected the spray point of high-tension electricity with being placed in one, and this ionic tube is communicated with an air inlet pipe, and air inlet pipe directly is communicated with neutral gas.
Said ionization tube comprises that an ionic tube is connected the spray point of high-tension electricity with being placed in one, and this ionic tube is communicated with an air inlet pipe, and the bottle or the pipe of liquid reagent is equipped with in air inlet pipe connection one, in bottle or pipe, feeds neutral gas in the reagent.
Said ionization tube is also claimed discharge tube; In be provided with the spray point that connects high-tension electricity, the needle body of spray point has insulating barrier, spray point is outward a sparge pipe; Sparge pipe is outward the carrier gas pipe; And spray point, sparge pipe, the coaxial placement of carrier gas pipe, the needle point of spray point stretches out the sparge pipe front end, and the sparge pipe front end stretches out carrier gas pipe front end.
Sparge pipe is established the fluid passage interface, in sparge pipe, imports reagent through the fluid passage interface; The carrier gas pipe is established the carrier gas passage interface, in the carrier gas pipe, imports carrier gas through the carrier gas passage interface.
Distance between the spray point needle point of ionization tube, the sparge pipe front end mouth of pipe, the carrier gas pipe front end mouth of pipe is adjustable.
The angle of said ionization tube and sample cell and distance are apart adjusted through the adjusting bracket that is provided with.
Adopt above design; The utility model normal pressure chemical extraction ionization source is through adopting spray point to ion reagent (air; Water vapours etc.) corona discharge generation ion a fluid stream and sample flow are collided in the space; Can be with nonpolar molecule in the sample even large biological molecule desorb, thereby thereby the determinand in the sample is extracted ionization makes determinand generation ionization, the ion of determinand produced.Adopt extraction ionization mode rather than simple surface desorption in addition, can realize that continuous sample introduction obtains the stable detection signal.The normal pressure chemical of the utility model extraction ionization source, compact conformation designs ingeniously, easy to use, can carry out the ionization analysis to various test sample; The utility model normal pressure chemical extraction MALDI-MS analytical method not only has the advantage of high sensitivity and high specific, and can select ion reagent to carry out selectivity and research reaction mechanism that ion molecule reaction improves reaction.Therefore, the biological sample, food, medicine, environmental sample etc. that are particularly suitable for complicacy of the method analyzed real-time.
Description of drawings
Fig. 1 is the basic comprising and the operation principle sketch map of the utility model normal pressure chemical extraction ionization source (EAPCI);
The basic comprising and the operation principle sketch map of Fig. 2 neutral desorb-normal pressure chemical extraction ionization source (ND-EAPCI) form for the utility model adopts;
Fig. 3 is the utility model normal pressure chemical extraction ionization source (EAPCI) another form basic comprising of ionization system and operation principle sketch map;
Embodiment
Specify the formation and the operation principle of the utility model normal pressure chemical extraction ionization source below in conjunction with accompanying drawing.
Fig. 1 shows the basic functional principle of normal pressure chemical extraction ionization source (being called for short EAPCI); Wherein passage 1 (ionization tube) is used to produce reagent ion stream for having the SDAPCI nozzle of spray point, and passage 2 (sample cell) is the DESI nozzle; Be used to spray sample flow; Two nozzles are with the common ionized space that points to of an angle, sample flow in this zone with reagent ion stream striking process in be ionized the formation ion beam, and then under electric field and suction function, enter the mouth and be introduced into mass spectrometer through MS.
With reference to above operation principle, in mass spectral analysis, the utility model normal pressure chemical extraction ionization source introduces as sample and ionization system uses, and it comprises sample drawing-in system and ionization system two parts.Fig. 2 illustrates a kind of form of the utility model; Ionization system (ionization tube) comprises ionic tube 5 and the spray point 6 that is placed in one and is connected high-tension electricity; Feed carrier gas in the ionic tube 5, gas can be directed to gas cylinder or air, and air inlet pipe 3 preferably connects a wet gas generator; This wet gas generator is the bottle of humidification reagent to be housed or to manage 4, and gas feeds and forms wet steam in the reagent again through air inlet pipe 3 introducing ionic tubes 5; Sample drawing-in system (sample cell) mainly comprises a sample inlet tube 1 and sample carrier gas pipe 2; Sample inlet tube 1 is a capillary with ionic tube 5; Two capillaries are an angle [alpha] and intersect oblique placement and point to ionization space jointly; Be fixed in respectively in adjusting bracket 7 and the adjusting bracket 8, the angle [alpha] of intersection and the mouth of pipe can be regulated through adjusting bracket with the distance b of angle beta, sample inlet tube 1 and the mass spectrometer injection port 9 of mass spectrometer injection port 9 apart from a and ionic tube 5.
In the utility model, but the neutral desorption apparatus of sample drawing-in system coupling is as shown in Figure 2, sample inlet tube 1 is connected the sample delivery line 12 of neutral desorption apparatus 10.Neutral desorption apparatus 10 can be with reference to the patent ZL200820233874.1 that declares before the utility model people; Under the air-flow effect of carrier gas breather pipe 11 composition to be measured on sample (article to be measured) surface 13 is being desorbed; Composition to be measured flow through sample delivery line 12 and sample inlet tube 1 are introduced ionization space and are carried out the ionization stepping of going forward side by side and go into mass spectrometer.
The normal pressure chemical extraction ionization source of the another kind of form of the utility model, its ionization system uses the discharge tube that has fluid passage, and is as shown in Figure 3; This discharge tube comprises spray point 21, sparge pipe 22 and carrier gas pipe 23; Sparge pipe 22 is a capillary with carrier gas pipe 23, and sparge pipe 22 is sleeved in the carrier gas pipe 23, and spray point 21 is sleeved in the sparge pipe 22; Spray point 21 needle bodies (remove tip portion) have insulating barrier with sparge pipe 22 in liquid isolate spray point 21, sparge pipe 22, the 23 coaxial placements of carrier gas pipe; The needle point of spray point 21 stretches out sparge pipe 22 front ends (apart from d), and sparge pipe 22 front ends stretch out carrier gas pipe 23 front ends (distance c); The carrier gas passage interface 25 that discharge tube is established high-tension electricity interface 26, the fluid passage interface 24 that is communicated with sparge pipe 22, is communicated with carrier gas pipe 23; Spray point 21 rear ends connect this high-tension electricity interface 26; In sparge pipe 22, import ionization reagents through fluid passage interface 24, in carrier gas pipe 23, import carrier gas through carrier gas passage interface 25; Can regulating apart from d of the distance c of two capillary exits and spray point needle point and sparge pipe 2 capillary exits, discharge tube is fixed in the adjusting bracket 7.The sample drawing-in system of the ionization source of this form can be the DESI nozzle, comprises a carrier gas pipe 28 and the sample cell 27 that loads in it.Certainly, also can use the sample drawing-in system of the neutral desorption apparatus of coupling of Fig. 1 b demonstration, repeat no more at this.
In the ionization process; Penetrate high-speed gas from carrier gas pipe 23 front ends; From sparge pipe 22 front end trickles; This high-speed gas makes the atomization of liquid form a large amount of droplets, and droplet was charged and form the ion flow (nitrogen, steam plasma, a large amount of ion beams of ejaculation also receive from the desiccation of carrier gas pipe 23 ejection gases) that sprays when simultaneously high-pressure made spray point 21 discharges; Ion flow directly with the sample gas collision of drawing by sample cell 27, the composition to be measured in the sample is by ionization and form ion beam and be introduced in mass spectrometer from mass spectrometer injection port 9 and carry out analyzing and testing.
Accordingly, use above-mentioned normal pressure chemical extraction ionization source and carry out mass spectral analysis multiple combination is arranged, the first combines neutral desorption apparatus 10 samplings to realize the neutral desorption atmospheric chemical extraction MALDI-MS of solid sample is analyzed (ND-EAPCI-MS).Shown in Fig. 1 b.With the lip-deep composition desorb to be measured of determinand (can be solid) and be transferred to the EAPCI ionization source and carry out ionization, the sample ions of formation imports mass spectrometer and carries out mass spectral analysis through neutral desorption apparatus.This ND-EAPCI-MS mass spectrometric analysis method may further comprise the steps:
Step 1: the outlet of the sample cell of neutral desorption apparatus (ND) is linked to each other with the sample introduction pipe of normal pressure chemical extraction ionization source (EAPCI), regulate and position that fixedly normal pressure chemical extracts ionization source (EAPCI) and mass spectrometer (MS) import;
Step 2: the sample cell inlet of neutral desorption apparatus is aimed at solid article to be checked surface, distance 5～12mm;
Step 3: to the air inlet pipe input neutral gas of neutral desorption apparatus, gas flow rate is 0～40psi;
Step 4: impose 3～5kV high pressure to normal pressure chemical extraction ionization source simultaneously and make sample ionization, feed nitrogen gas in the ionic tube, gas flow rate is 20psi;
Step 5: open the mass spectrometer scanning system, obtain testing result.
When using discharge tube shown in Figure 3 to produce reagent ion stream, when adding high pressure in the step 4, in sparge pipe, add liquid reagent, flow rate of liquid is 5 μ L/min; In the carrier gas pipe, feed neutral gas (nitrogen), gas flow rate is 15psi.
Carrier gas of mentioning among this paper or neutral gas are for being selected from innocuous gas such as water vapour, nitrogen, air.The reagent of mentioning is like bottle or manage one or more the mixture that the reagent (ionization reagents) that imports in liquid reagent (humidification reagent) or the sparge pipe 22 in 4 can be selected reagent such as water, methyl alcohol, acetic acid, ammoniacal liquor for use.
Using the utility model ionization source can carry out normal pressure chemical extraction MALDI-MS (EAPCI-MS) analyzing and testing to the nonpolar molecule sample explosive in nonpolar molecule standard items, the complicated substrate, the big molecule of bioprotein, has obtained good result.But the ND-EAPCI-MS through combining neutral desorption apparatus is the metabolin of remote analysis plant also.
Claims (9)
1. a normal pressure chemical extracts ionization source; Be provided with ionization tube and sample cell; Ionization tube and sample cell point to ionized space jointly with an angle and the oblique placement of a spacing and port; It is characterized in that: sample cell comprises a sample inlet tube and sample carrier gas pipe, imports gas or fluid sample in the sample inlet tube or connects the sample delivery line of a neutral desorption apparatus.
2. normal pressure chemical extraction ionization source according to claim 1 is characterized in that said ionization tube comprises that an ionic tube is connected the spray point of high-tension electricity with being placed in one, and this ionic tube is communicated with an air inlet pipe, and air inlet pipe directly is communicated with neutral gas.
3. normal pressure chemical extraction ionization source according to claim 1; It is characterized in that; Said ionization tube comprises that an ionic tube is connected the spray point of high-tension electricity with being placed in one; This ionic tube is communicated with an air inlet pipe, and the bottle or the pipe of liquid reagent is equipped with in air inlet pipe connection one, feeds neutral gas in the interior reagent of bottle or pipe.
4. normal pressure chemical extraction ionization source according to claim 1 is characterized in that said ionization tube is made up of spray point, sparge pipe and the carrier gas pipe of coaxial placement; Spray point connects high-tension electricity; Its needle body has insulating barrier, and spray point is outward a sparge pipe, and sparge pipe is outward the carrier gas pipe.
5. normal pressure chemical extraction ionization source according to claim 4 is characterized in that the needle point of said spray point stretches out the sparge pipe front end, and the sparge pipe front end stretches out carrier gas pipe front end.
6. normal pressure chemical extraction ionization source according to claim 4, it is characterized in that: sparge pipe is established the fluid passage interface that is used to import reagent, and the carrier gas pipe is established the carrier gas passage interface that is used to import gas.
7. according to claim 4 or 5 or 6 described normal pressure chemical extraction ionization sources, it is characterized in that: the distance between the spray point needle point of described ionization tube, the sparge pipe front end mouth of pipe, the carrier gas pipe front end mouth of pipe is adjustable.
8. according to the arbitrary described normal pressure chemical extraction ionization source of claim 1 to 6, it is characterized in that: said ionization tube and sample cell are positioned on the adjusting bracket, its angle and adjustable apart.
9. want 7 described normal pressure chemical extraction ionization sources according to right, it is characterized in that: said ionization tube and sample cell are positioned on the adjusting bracket, its angle and adjustable apart.
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| CN2011202368912U CN202120862U (en) | 2010-07-06 | 2011-07-06 | Normal pressure chemical extraction ionization source |
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| CN201010226321.5 | 2010-07-06 | ||
| CN201010226321 | 2010-07-06 | ||
| CN2011202368912U CN202120862U (en) | 2010-07-06 | 2011-07-06 | Normal pressure chemical extraction ionization source |
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| CN2011101886800A Pending CN102280347A (en) | 2010-07-06 | 2011-07-06 | Normal pressure chemical extraction ionization source and normal pressure extraction ionization mass spectrometry method |
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| CN104538276A (en) * | 2014-12-26 | 2015-04-22 | 宁波大学 | Ion source soft ionization device and method under barometric pressure |
| CN105588872A (en) * | 2016-03-02 | 2016-05-18 | 中国科学技术大学 | Quick on-line atmospheric photo ionization mass spectrum device for effective constituent in complex substrate |
| CN115266896A (en) * | 2022-09-26 | 2022-11-01 | 宁波华仪宁创智能科技有限公司 | Biological sample analysis system and method |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1206493A (en) * | 1996-08-29 | 1999-01-27 | 日本钢管株式会社 | Laser ionization mass spectroscope and mass spectrometric analysis method |
| CN101073137A (en) * | 2004-03-30 | 2007-11-14 | 普渡研究基金会 | Method and system for desorption electrospray ionization |
| FR2896585B1 (en) * | 2006-01-20 | 2008-12-05 | Commissariat Energie Atomique | INTRODUCTION OF ADDITIVES FOR AN ATMOSPHERIC PRESSURE IONIZATION INTERFACE INTO A SPECTROMETER |
| US20080179511A1 (en) * | 2007-01-31 | 2008-07-31 | Huanwen Chen | Microspray liquid-liquid extractive ionization device |
-
2011
- 2011-07-06 CN CN2011202368912U patent/CN202120862U/en not_active Expired - Lifetime
- 2011-07-06 CN CN2011101886800A patent/CN102280347A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104538276A (en) * | 2014-12-26 | 2015-04-22 | 宁波大学 | Ion source soft ionization device and method under barometric pressure |
| CN105588872A (en) * | 2016-03-02 | 2016-05-18 | 中国科学技术大学 | Quick on-line atmospheric photo ionization mass spectrum device for effective constituent in complex substrate |
| CN115266896A (en) * | 2022-09-26 | 2022-11-01 | 宁波华仪宁创智能科技有限公司 | Biological sample analysis system and method |
| CN115266896B (en) * | 2022-09-26 | 2023-01-13 | 宁波华仪宁创智能科技有限公司 | Biological sample analysis system and method |
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| CN102280347A (en) | 2011-12-14 |
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Legal Events
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200520 Address after: 330038 R & D center of electromechanical Industrial Science and Technology Park, No. 88, Dingxiang Road, Nanchang Economic and Technological Development Zone, Nanchang City, Jiangxi Province Patentee after: Jiangxi Zhengpu Yihe Technology Co., Ltd Address before: 344000 No. 56, Xuefu Road, Fuzhou, Jiangxi Patentee before: EAST CHINA INSTITUTE OF TECHNOLOGY |
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| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20120118 |