CN202111053U - Surface extraction chemical ionization source - Google Patents

Surface extraction chemical ionization source Download PDF

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Publication number
CN202111053U
CN202111053U CN201120235815XU CN201120235815U CN202111053U CN 202111053 U CN202111053 U CN 202111053U CN 201120235815X U CN201120235815X U CN 201120235815XU CN 201120235815 U CN201120235815 U CN 201120235815U CN 202111053 U CN202111053 U CN 202111053U
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China
Prior art keywords
tube
ionization
carrier gas
ionization source
pipe
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Expired - Lifetime
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CN201120235815XU
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Chinese (zh)
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陈焕文
胡斌
张兴磊
欧阳永中
肖赛金
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East China Institute of Technology
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East China Institute of Technology
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Abstract

A surface extraction chemical ionization source comprises an ionization tube and a sample bearing platform, the ionization tube is provided with a discharge needle inside, a liquid spraying tube is arranged outside the discharge needle, a carrying gas tube is arranged outside the liquid spraying tube, and the discharge needle, the liquid spraying tube and the carrying gas tube are coaxially arranged; the needle point of the discharge needle protrudes from the front end of the liquid spraying tube, the front end of the liquid spraying tube protrudes from the front end of the carrying gas tube, distances of the needle point of the discharge needle, the mouth of the front end of the liquid tube and the mouth of the front end of the carrying gas tube are adjustable. Carrying gas is introduced to the carrying gas tube, an extraction reagent is added to the liquid spraying tube, the discharge needle is connected to a high voltage, an article to be tested is placed on the surface of the bearing platform, a substance to be tested on surface of the article is extracted by using a carrying gas atomization extractant and is desorbed, at the same time, the discharge needle discharges an ionization reagent to prompt the ionization of the substance to be tested for mass spectrometry. The surface extraction chemical ionization source is especially suitable for realtimely and rapidly analyzing complicated biological samples, foods, medicines and environment samples.

Description

A kind of surperficial extraction chemistry ionization source
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 surperficial extraction chemistry ionization source device 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; Owing to adopt air-flow desorb surface, on the complicated substrate surface, combining firm material (like protein and other) to be difficult to desorption ionization.
The utility model content
The technical problem that the utility model solves is; Solve the material that the surface chemistry ionization source can not desorption ionization shows that adhesion on the sample is firm and the problem of surface biomacromolecule sample; Provide a kind of assembling simple, low cost of manufacture, Ionization Efficiency is high; Desorption efficiency is high, the surperficial extraction chemistry ionization source that detection sensitivity is high.
The surperficial extraction chemistry ionization source of the utility model comprises ionization tube and sample plummer, and the ionization tube front end points to plummer at a certain angle; Be provided with spray point in the said ionization tube; Spray point is outward a sparge pipe, and sparge pipe is outward the carrier gas pipe, and spray point, sparge pipe, the coaxial placement of carrier gas pipe.
Wherein: 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.
Distance between the spray point needle point of described ionization tube, the liquid line front end mouth of pipe, the carrier gas pipe front end mouth of pipe is adjustable.
Discharge tube is established the high-tension electricity interface, and the spray point rear end connects high-tension electricity through this high-tension electricity interface.
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.
Spray point in the said ionization tube has insulating barrier.
The distance of said ionization tube and plummer and adjustable angle.
Adopt above design; The utility model surface extraction chemistry ionization source produces ion a fluid stream and sample flow at surface collision through adopting spray point to the reagent corona discharge; Thereby make determinand generation ionization thereby the determinand in the sample is extracted ionization, produce the ion flow of determinand.Owing to adopt the spray point corona discharge to have very high ionizing power, can be with nonpolar molecule even large biological molecule ionization, this ionization source structure is compact, designs ingeniously, easy to use, can carry out the ionization analysis to various test sample; The biological sample, food, medicine, environmental sample etc. that utilize the utility model ionization source to be particularly suitable for complicacy are analyzed real-time.
Description of drawings
Fig. 1 is the basic comprising and the operation principle sketch map of the utility model surface extraction chemistry ionization source;
Fig. 2 is a discharge vessel end bilge construction enlarged drawing among Fig. 1.
Embodiment
Specify the formation and the operation principle of the utility model surface extraction chemistry ionization source below in conjunction with accompanying drawing.
Fig. 1 shows the basic comprising and the operation principle of the utility model surface extraction chemistry ionization source.In mass spectral analysis; The utility model surface extraction chemistry ionization source introduces as sample simultaneously and ionization system uses; It comprises discharge tube, sample plummer and framework; Sample is introduced and to be placed in sample plummer 6 surfaces or the sample cell by sample (article to be measured), and sample plummer 6 is fixed in the framework (among the figure not display frame), about the sample plummer can carry out, up and down, the moving and the location of orientation such as front and back; Available sample plummer and framework etc. can be with reference to the contents of introducing among the ZL200710307112.1.In the utility model, discharge tube is through particular design, and it comprises spray point 1, sparge pipe 2 and carrier gas pipe 3; Sparge pipe 2 is a capillary with carrier gas pipe 3; Referring to Fig. 2, sparge pipe 2 is sleeved in the carrier gas pipe 3, and spray point 1 is sleeved in the sparge pipe 2; Spray point 1 needle body have insulating barrier with sparge pipe in liquid isolate spray point 1, sparge pipe 2, the 3 coaxial placements of carrier gas pipe; The needle point of spray point 1 stretches out sparge pipe 2 front ends (apart from d), and sparge pipe 2 front ends stretch out carrier gas pipe 3 front ends (distance c); The carrier gas passage interface 5 that discharge tube is established high-tension electricity interface, the fluid passage interface 4 that is communicated with sparge pipe 2, is communicated with carrier gas pipe 3; Spray point 1 rear end connects this high-tension electricity interface; In sparge pipe 2, import reagent through fluid passage interface 4, in carrier gas pipe 3, import carrier gas through carrier gas passage interface 5; 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 also are fixed in the framework also adjustable.Sparge pipe 2 can pass through frame adjustment with the angle [alpha] of sample plummer 6 inclinations with apart from a and sample plummer 6 with the angle beta and the distance b of mass spectrum injection port 7.
When the utility model surface extraction chemistry ionization source uses; In the sample ionization process; Penetrate high-speed gas from carrier gas pipe 3 front ends, from sparge pipe 2 front end trickles, this high-speed gas makes the atomization of liquid form a large amount of droplets; Droplet was charged and form the ion beam that sprays when simultaneously high-pressure made spray point 1 discharge; Ion beam directly with collide by the sample on the sample plummer 6, take place to merge extraction and desorb ionization reaction with material on the sample surfaces, under the effect of ionization source high velocity air and high-tension electricity, the test substance in the sample is carried out desorption ionization like this; And receive the purging desiccation of gas, the determinand in the sample is by ionization and be incorporated into mass spectrometer and carry out analyzing and testing.
During surface extraction chemistry ionization source uses; Import carrier gas in the carrier gas pipe, add extraction agent in the sparge pipe, spray point connects high-tension electricity; Article to be measured place on the carrier-table surface; Through carrier gas atomizing extractant extraction lip-deep determinand of article and desorb, simultaneously, spray point discharge ionization reagents is also impelled the determinand ionization and is able to carry out mass spectral analysis.Therefore; Can utilize the utility model surface extraction chemistry ionization source as mass spectrometric sample drawing-in system and ionization system; The reagent ion stream of ionization tube ejection is implemented wherein determinand of collision and extraction and desorb to the article to be checked that directly are positioned over carrier-table surface, forms the sample ions bundle and gets into mass spectrometer and carry out mass spectral analysis.
Show through concrete detection instance; Use the utility model and carry out the analysis of surperficial extraction chemistry MALDI-MS; Direct detection to nonpolar molecule benzene, naphthalene; To the desorption ionization of high molecular weight protein lysozyme, insulin, detect and analyze the detection of phenylalanine in detection and the blood of hemoglobin in the detection, blood of lysozyme in detection like lysozyme in the saliva, the milk in the complicated substrate biological sample, all obtained good result.

Claims (8)

1. a surperficial extraction chemistry ionization source comprises ionization tube and sample plummer, and the ionization tube front end points to plummer with an angle; It is characterized in that, be provided with spray point in the said ionization tube, 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.
2. surperficial extraction chemistry ionization source according to claim 1, it is characterized in that: 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.
3. surperficial extraction chemistry ionization source according to claim 2 is characterized in that: the distance between the spray point needle point of said ionization tube, the liquid line front end mouth of pipe, the carrier gas pipe front end mouth of pipe is adjustable.
4. surperficial extraction chemistry ionization source according to claim 2 is characterized in that: the distance of said ionization tube and plummer and adjustable angle.
5. according to claim 1 or 2 or 3 or 4 described surperficial extraction chemistry ionization sources, it is characterized in that: the spray point in the sparge pipe has insulating barrier.
6. surperficial extraction chemistry ionization source according to claim 5, it is characterized in that: discharge tube is established the high-tension electricity interface, and the spray point rear end connects high-tension electricity through this high-tension electricity interface.
7. surperficial extraction chemistry ionization source according to claim 5 is characterized in that: sparge pipe is established the fluid passage interface that is used to import reagent; The carrier gas pipe is established the carrier gas passage interface that is used to import gas.
8. surperficial extraction chemistry ionization source according to claim 6 is characterized in that: it is characterized in that: sparge pipe is established the fluid passage interface that is used to import reagent; The carrier gas pipe is established the carrier gas passage interface that is used to import gas.
CN201120235815XU 2010-07-06 2011-07-06 Surface extraction chemical ionization source Expired - Lifetime CN202111053U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102928498A (en) * 2012-11-06 2013-02-13 东华理工大学 Extractive electrospray ionization mass spectrometry method for inside of tissue sample
CN107430048A (en) * 2015-01-12 2017-12-01 艾德维昂股份有限公司 Surface extractions interface
CN108152360A (en) * 2018-02-08 2018-06-12 中国检验检疫科学研究院 The dielectric barrier discharge ionization mass spectrometry method of perfluorochemical in textile

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CN104037047B (en) * 2014-06-12 2016-04-20 浙江好创生物技术有限公司 A kind of method preparing molecule adduction isotope ion
CN107121487B (en) * 2017-07-05 2019-10-01 中国检验检疫科学研究院 A kind of normal pressure velocity of sound electrospray ionization device and its application
CN108414609B (en) * 2018-02-05 2023-09-22 吉林大学 Online mass spectrum detection device for nutrient component change process in traditional Chinese medicine steaming process
CN113933378A (en) * 2021-09-01 2022-01-14 南水北调中线干线工程建设管理局河北分局 Water body characteristic value analysis method
CN113838738A (en) * 2021-09-14 2021-12-24 清华大学深圳国际研究生院 Mass spectrum combined multi-channel electrospray micro-fluidic chip ion source

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US7544933B2 (en) * 2006-01-17 2009-06-09 Purdue Research Foundation Method and system for desorption atmospheric pressure chemical ionization
CN101211741A (en) * 2006-12-28 2008-07-02 东华理工学院 Mass spectrometer multifunctional multichannel ion source
CN101201335B (en) * 2006-12-29 2011-06-15 东华理工学院 Surface desorption atmospheric chemical ionization source of mass spectrometer
WO2009124298A2 (en) * 2008-04-04 2009-10-08 Agilent Technologies, Inc. Ion sources for improved ionization

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102928498A (en) * 2012-11-06 2013-02-13 东华理工大学 Extractive electrospray ionization mass spectrometry method for inside of tissue sample
CN107430048A (en) * 2015-01-12 2017-12-01 艾德维昂股份有限公司 Surface extractions interface
CN108152360A (en) * 2018-02-08 2018-06-12 中国检验检疫科学研究院 The dielectric barrier discharge ionization mass spectrometry method of perfluorochemical in textile
CN108152360B (en) * 2018-02-08 2020-12-11 中国检验检疫科学研究院 Dielectric barrier discharge ionization mass spectrometry analysis method for perfluorinated compounds in textiles

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Granted publication date: 20120111

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