WO2006054911A1 - Procede de desorption de molecules induite par laser et dispositif de sa mise en oeuvre - Google Patents

Procede de desorption de molecules induite par laser et dispositif de sa mise en oeuvre Download PDF

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Publication number
WO2006054911A1
WO2006054911A1 PCT/RU2004/000451 RU2004000451W WO2006054911A1 WO 2006054911 A1 WO2006054911 A1 WO 2006054911A1 RU 2004000451 W RU2004000451 W RU 2004000451W WO 2006054911 A1 WO2006054911 A1 WO 2006054911A1
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WIPO (PCT)
Prior art keywords
vacuum
region
substrate
molecules
vacuum region
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PCT/RU2004/000451
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English (en)
Russian (ru)
Inventor
Yuri Konstantinovich Nizienko
Original Assignee
Yuri Konstantinovich Nizienko
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Filing date
Publication date
Application filed by Yuri Konstantinovich Nizienko filed Critical Yuri Konstantinovich Nizienko
Priority to PCT/RU2004/000451 priority Critical patent/WO2006054911A1/fr
Publication of WO2006054911A1 publication Critical patent/WO2006054911A1/fr

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
    • H01J49/161—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission using photoionisation, e.g. by laser
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/2813—Producing thin layers of samples on a substrate, e.g. smearing, spinning-on
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
    • G01N2001/045—Laser ablation; Microwave vaporisation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/2813—Producing thin layers of samples on a substrate, e.g. smearing, spinning-on
    • G01N2001/2826—Collecting by adsorption or absorption

Definitions

  • the invention relates to the field of mass spectrometry technology and can be used mainly in medicine and molecular biology, as well as in other fields of science and technology, for example, in the State Anti-Terrorism Program by providing highly sensitive control and / or detection of targets (for control and / or detection) of substances at the biomolecular level.
  • targets for control and / or detection
  • substances at the biomolecular level for example: drugs, and / or explosives, and / or other substances derived from aromatic hydrocarbons widely used in the national economy.
  • the prior art method of laser-induced desorption of the molecules of the analyte from the adsorbing surface of the substrate (silicon wafer placed in the vacuum chamber of the mass spectrometer / mass analyzer /), as well as a device for its implementation, which consists in the fact that on the absorbent surface of the substrate form a layer of the substance under study by any method known in the art (for example, by deposition from an external medium relative to the vacuum region) with the subsequent ionization of atomic-molecular structures substance, as well as their directed desorption into the vacuum region.
  • the mentioned processes of ionization and desorption are carried out under the influence of laser radiation pulses on the region of the test substance, by means of the light energy of which energy of a different physical form (in particular, thermal energy) is induced in the zone of the test substance.
  • the latter i.e., the induced thermal energy
  • the aforementioned processes of ionization and desorption in this case, thermal
  • JOURNAL OF CHEMICAL PHYSICS, VOLUME 115, NUMBER 4, 22 JULY 2001, PAGE 1891-1901 JOURNAL OF CHEMICAL PHYSICS, VOLUME 115, NUMBER 4, 22 JULY 2001, PAGE 1891-1901.
  • the main disadvantage of the solutions known from the prior art is that the substrate with the test substance must be placed in the evacuation area before the start of the process cycle of the directed desorption of the molecules of the test substance (i.e., before the process of evacuation of the gaseous medium from the vacuum chamber of the device).
  • the substrate with the test substance must be placed in the evacuation area before the start of the process cycle of the directed desorption of the molecules of the test substance (i.e., before the process of evacuation of the gaseous medium from the vacuum chamber of the device).
  • part of the atomic-molecular structures of the test substance spontaneously desorb to the evacuated region and settle on the walls of the device’s vacuum chamber.
  • the quantitative composition of the test substance deposited on the absorbent surface of the substrate varies significantly, and, accordingly, the results of the rapid analysis with respect to the concentration of this substance (for example, in the external environment) will differ significantly from its real concentration in the environment.
  • the disadvantages of the data known from the prior art, method and device for its implementation include the fact that as a result of increasing the energy of laser radiation (to ensure complete desorption of atomic-molecular structures deposited on the absorbent surface of the substrate) on the test substance (and as a result, on the material of the absorbent substrate in the location region of the test substance), together with the desorption of the test substance, the desorption of the substrate material occurs, which has a negative effect on the results of the study and allows one to determine (by long and laborious processing of the experimental results) only the qualitative composition of the test substance (with a certain degree of certainty), and not the quantitative content ( ratio) of the atomic-molecular / chemical / structures included in it, which is the most important and valuable information when conducting this kind of exp c- analysis of the test substance for the purposes of identification and concentration determination, for example, in the outer, with respect to the vacuum region medium.
  • the technical task of the claimed method of laser-induced desorption of the molecules of the analyte from the absorbent surface of the substrate is to provide the possibility in the process of express analysis of the test substance to obtain information not only about the reliable qualitative composition of this substance (by reducing the energy of laser radiation and, accordingly, exclusion of desorption into the vacuum region of atomic-molecular structures of the substrate material), but also about reliable quantitative ootnoshenii (content) of its constituent chemical components (atomic-molecular structures) in an external (relative to the vacuum region) medium.
  • At least one stripping zone of the absorbent surface of the substrate is placed relative to the vacuum region so that it is precisely this zone of the absorbent surface that is located in the vacuum region, so that the vacuum region communicates with the external medium through a discrete physical and technological channel, said at least one desorbing zone of the absorbent surface of the substrate is tightly mated to the outer boundary of the vacuum region at the location of said about the physical-technological channel with the possibility of cyclic movement of at least part of the absorbent surface of the substrate relative to the channel according to a given program.
  • the wavelength range of the used laser radiation from the condition of ensuring maximum energy absorption of this radiation in the surface layer of the absorbent substrate, the thickness of which is comparable with the thickness of the monolayer of the molecules of the substance under study adsorbed from the external medium relative to the vacuum region.
  • the destabilization of pressure in the vacuum region arising in it due to the presence of the mentioned physical-technological channel can compensate by continuous regulated pumping of the gaseous medium from the mentioned area during the full technological cycle of the desorption process.
  • the task in relation to the object of the invention "property" is solved by the fact that in the device for laser-induced desorption of molecules, including a vacuum chamber, a substrate with the molecules of the studied substance deposited on its adsorbing surface, as well as a stand-alone ionization means of these molecules, made in the form of a source laser radiation, in which the absorbent surface of the substrate is placed relative to the vacuum region of the vacuum chamber with the possibility of directional desorption of ionized moles at least one zone of the absorbent surface of the substrate, from which the ionized molecules of the analyte are desorbed, into the vacuum region, the rest part of the area of the absorbent surface of the substrate is located outside the aforementioned vacuum region with the possibility of its relative movement but the last and continuous adsorption of the molecules of the substance under study from the external medium relative to the vacuum region, while the laser radiation source is placed with the possibility of concentration of its energy on the said zone of the absorbent surface located in the vacuum region.
  • the invention is illustrated by graphic materials on which a general diagram of a device for implementing the inventive method of laser-induced desorption of molecules (mainly biomolecules) in vacuum is presented.
  • the method of laser-induced desorption of molecules is as follows.
  • Laser-induced desorption of molecules consists in the fact that through special processing (for example, etching or ablation) of the surface of the substrate (for example, silicon) on it form, respectively, an oxide film or a rough surface layer (absorbent surface). On such a surface, the settled biomolecules of the test substance are easily ionized and ablated by means of energy exposure to them by laser radiation.
  • the rest of the area of the adsorbing surface 4 of the substrate 5 is located outside the vacuum region 1 with the possibility of its movement relative to the latter (i.e., vacuum region 1) and continuous adsorption of the molecules of the substance under study from the external medium relative to the vacuum region 1.
  • the energy of a stand-alone ionization means activating the desorption of ionized molecules 3 of the test substance is directed from the vacuum region 1 with the possibility of its concentration on the aforementioned currently located in the vacuum region 1 zone of the adsorbing surface 4 of the substrate 5.
  • the arrangement of at least one desorbing zone of the adsorbing surface 4 of the substrate 5 with respect to the vacuum region 1 so that precisely this zone of the absorbing surface 4 is located in the vacuum region 1 can be accomplished, for example, by means of the fact that the vacuum region 1 is in communication with the external environment by discrete physical and technological channel 6.
  • the at least one desorbing zone of the adsorbing surface 4 of the substrate 5 is tightly mated with the outer boundary of the vacuum region 1 at the location the said physical-technological channel 6.
  • the density of the aforementioned conjugation is regulated by the possibility of cyclic movement of at least part of the absorbent surface 4 of the substrate 5 relative to the said channel 6 according to a predetermined program.
  • the wavelength range of the used laser radiation from the condition of ensuring maximum energy absorption of this radiation in the surface layer of the absorbent substrate 4, the thickness which is commensurate with the thickness of the monolayer adsorbed from the external, relative to region 1 of the vacuum, medium of the molecules of the substance under study. This eliminates the possibility of desorption of the atomic-molecular structures of the material of the substrate 5 in the region 1 of the vacuum during the technological cycle of rapid analysis of the test substance.
  • the destabilization of pressure in the vacuum region 1 arising in it due to the presence of the aforementioned physical and technological channel 6 can be compensated by continuously regulated pumping of the gaseous medium from the mentioned region 1 during the entire technological cycle of the desorption process (i.e., the rapid analysis of the studied substances). This improves the reliability of the results of the express analysis of the analyte, since in this case the full technological cycle of the express analysis is carried out under the same conditions that are optimal for the given cycle.
  • the zone of the adsorbing surface 4 of the substrate 5, which is opposite the physical-technological channel 6, essentially belongs to two regions simultaneously: region 1 of the vacuum and the external (relative to region 1 of the vacuum) medium, for example the atmosphere (i.e., the air). Since it is only necessary to shift the substrate 5 relative to the mentioned physical-technological channel 6 and the corresponding zone of the adsorbing surface 4 of the substrate 5 will already be outside the vacuum region 1, that is, in the atmosphere and “breathing” air in exactly the same mode as any other part of the absorbent surface 4 of the substrate 5, located in the air.
  • the troughs (lagoons) of the adsorbent surface 4 of the substrate 5 will retain the initial concentration of molecules (for example, biomolecules) for the external environment (atmosphere).
  • the absorbent surface 4 of the substrate 5 should not be mirror polished, i.e. must have a certain roughness, and, in addition, with a reasonable effort should be coupled with the outer boundary of the vacuum region 1 to enable movement relative to the physical-technological channel 6, mainly at a constant speed.
  • almost the entire absorbent surface 4 of the substrate 5 will be in the air (except for the zone that is located strictly opposite the physical-technological channel 6). It is from this zone that the ionized atomic-molecular structures (for example, biomolecules) of the studied substance are desorbed into the vacuum region 1 as a result of the regulated energy impact on the said zone by a focused laser beam.
  • the claimed method implements the above-described effect of intensification of ionization of the molecules of the investigated substance due to their constant interaction with the aqueous medium (atmospheric moisture). That is, moisture (several monolayers of water) is always present on the absorbent surface 4 of the substrate 5, which is in the atmosphere, which helps the molecules of the substance under study to ionize with high basicity, because when laser radiation heats the complexes of biomolecules with water, the desorption of biomolecules with attached by protons from water molecules. Thus, desorption of the ionized molecules 3 of the test substance from the absorbent surface 4 of the substrate 5 occurs.
  • the aqueous medium atmospheric moisture
  • water molecules are proton donors with respect to the molecules of the test substance, because give them part of their charge, ionizing the latter.
  • moisture water molecules practically does not penetrate into region 1 of the vacuum in the process cycle of the process of rapid analysis of the test substance.
  • a device for laser-induced desorption of molecules includes a vacuum chamber 7, a substrate 5 with 4 molecules of an analyte deposited on its adsorbing surface, as well as a stand-alone ionization means of the above molecules, made in the form of a laser radiation source 2.
  • the absorbent surface 4 of the substrate 5 is placed relative to the vacuum region 1 of the vacuum chamber 7 with the possibility of directed desorption of the ionized molecules 3 of the test substance from the absorbent surface 4 into the vacuum region 1 by means of concentrated energy exposure to the laser radiation source 2.
  • only at least one zone of the adsorbing surface 4 of the substrate 5 is placed, from which the ionized molecules 3 of the test substance are desorbed into the vacuum region 1.
  • the rest of the area of the adsorbing surface 4 of the substrate 5 is located outside the mentioned region 1 of the vacuum with the possibility of its movement relative to the last and continuous adsorption of molecules of the test substance from an external, relative to region 1 of the vacuum medium.
  • the laser radiation source 2 is arranged to concentrate its energy (i.e., focus the laser beam, for example, using a focusing lenses 8) on said adsorbed surface 4 of substrate 5 located in the vacuum region 1.
  • a focused laser beam activates and ionizes the molecules of the investigated substance adsorbed by the corresponding zone of the absorbent surface 4 of the substrate 5 from the external (relative to the vacuum region 1). Moreover, the energy impact of laser radiation is carried out only on that area of the absorbent surface 4 of the substrate 5, which is located strictly opposite the technological hole 9.
  • the source of laser radiation 2 is advisable to place outside the vacuum region 1 of the vacuum chamber 7, and the laser beam can be directed to the technological hole 9 (followed by focusing on the corresponding zone of the absorbent surface 4 of the substrate 5 by means of a lens 8), for example, by means of mirrors 11.
  • a specific area of the absorbent surface 4 of the substrate 5 is initiated by the focused laser beam, in fact, its heating due to the absorption of radiation energy only by the surface (adsorbing) layer of the substrate 5 (due to the choice of a certain wavelength), the thickness of which is essentially commensurate mA with a thickness of a monolayer of adsorbed molecules from the external environment.
  • thermionic emission of ionized molecules 3 occurs due to the high temperature of the surface layer, which includes mainly the molecules of the test substance.
  • the radiation energy is absorbed by the small mass of the corresponding desorbing zone of the adsorbing surface 4 of the substrate 5, as a result of which a high temperature is generated in this zone, which ensures thermal ionization and ablation of the ionized molecules 3 of the test substance in the vacuum region 1.
  • a field is formed in the vacuum chamber 7, which draws the ionized ablated molecules 3 of the test substance into the vacuum region 1 and further, by the time of flight, the mass of these molecules is analyzed, and their concentration in the external medium is analyzed by the number.
  • a pulsed-periodic neodymium laser was used with the output radiation converted to the third harmonic, having the following parameters with the following parameters: radiation wavelength - 35 nm, pulse energy up to 50 mJ, beam cross section diameter ⁇ l, 0 mm, pulse duration was ⁇ l, 5 nsec.
  • the pressure in the vacuum region 1 of the vacuum chamber 7 of the mass transit analyzer was about 10 " mm Hg.
  • the diameter of the process hole 9 in the wall of the vacuum chamber 7 was" 30 ⁇ m.
  • the claimed inventions can find wide application in various fields of science and technology, mainly, the claimed method of desorption of molecules (for example, biomolecules) of a test substance from an absorbent substrate (as well as a device for its implementation) can be used in medicine and molecular biology, and also in other areas, for example, in the State program of antiterrorist activities by providing highly sensitive control and / or detection of targets (for For and / or detection) of substances at the biomolecular level.
  • targets for For and / or detection

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Plasma & Fusion (AREA)
  • Engineering & Computer Science (AREA)
  • Optics & Photonics (AREA)
  • Electron Tubes For Measurement (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

L'invention concerne des procédés et moyens de désorption de molécules induite par laser et peut s'utiliser pour déterminer la composition quantitative et qualitative d'une substance. Le procédé consiste en ce qui suit: au moyen d'une source de rayonnement laser (2) on effectue dans une région sous vide (1) la désorption des molécules d'une substance examinée à partir d'une surface adsorbante (4) d'un substrat (5), à destination (1) du vide. Dans une région sous vide (1) on dispose une zone de surface adsorbante (4) à partir de laquelle on effectue la désorption des molécules de substance examinée à destination (1) du vide. Le reste de la zone de surface adsorbante (4) est disposé en dehors de la région sous vide (1), de manière à pouvoir le déplacer par rapport à cette dernière et à assurer l'adsorption des molécules de substance examinée à partir de l'environnement. A cet effet, on fait communiquer la région sous vide (1) avec l'environnement au moyen d'un canal technique (6). L'énergie du rayonnement laser est concentrée sur une zone de surface adsorbante (4) disposée dans la région sous vide (1). Le dispositif comprend une chambre à vide (7), un substrat (5) avec des molécules de substance examinée, déposées sur sa surface adsorbante (4), et une source de rayonnement laser (2). La surface adsorbante (4) est disposée par rapport à la région sous vide (1) avec une possibilité de désorption de molécules ionisées (3) de substance examinée avec la surface adsorbante (4) dans la région sous vide (1), au moyen de l'énergie du rayonnement laser. Dans la région sous vide (1) on a disposé une zone de surface adsorbante (4), qui désorbe à un moment donné à destination de la région sous vide (1). Le reste de la zone de surface adsorbante (4) est situé en dehors de la région sous vide (1), avec possibilité de déplacement et d'adsorption des molécules de substance examinée à partir de l'environnement. A cet effet, on fait communiquer la chambre à vide (7) avec l'environnement au moyen d'un orifice technique (9). La source de rayonnement laser (2) est disposée avec la possibilité de concentration de son énergie sur une zone de surface adsorbante (4) située dans la région sous vide (1).
PCT/RU2004/000451 2004-11-15 2004-11-15 Procede de desorption de molecules induite par laser et dispositif de sa mise en oeuvre WO2006054911A1 (fr)

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PCT/RU2004/000451 WO2006054911A1 (fr) 2004-11-15 2004-11-15 Procede de desorption de molecules induite par laser et dispositif de sa mise en oeuvre

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4006381A1 (fr) 2009-04-16 2022-06-01 Fallbrook Intellectual Property Company LLC Ensemble stator et mécanisme de changement de vitesse pour transmission variable en continu

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU966792A1 (ru) * 1980-02-13 1982-10-15 Институт органической химии им.Н.Д.Зелинского АН СССР Способ анализа следовых количеств органических соединений на поверхности твердых тел
DE4017804A1 (de) * 1989-08-22 1991-03-14 Finnigan Mat Gmbh Verfahren und vorrichtung zur laserdesorption von analytmolekuelionen, insbesondere von biomolekuelen
DE19617011A1 (de) * 1996-04-27 1997-11-06 Bruker Franzen Analytik Gmbh Verfahren zur matrixunterstützten ionisierenden Laserdesorption
RU2099811C1 (ru) * 1988-07-08 1997-12-20 Колдрен Лимитед Партпершип Способ удаления поверхностных примесей с поверхности подложки и устройство для его осуществления
RU2124783C1 (ru) * 1994-06-07 1999-01-10 Александр Алексеевич Макаров Способ анализа макромолекул биополимеров

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU966792A1 (ru) * 1980-02-13 1982-10-15 Институт органической химии им.Н.Д.Зелинского АН СССР Способ анализа следовых количеств органических соединений на поверхности твердых тел
RU2099811C1 (ru) * 1988-07-08 1997-12-20 Колдрен Лимитед Партпершип Способ удаления поверхностных примесей с поверхности подложки и устройство для его осуществления
DE4017804A1 (de) * 1989-08-22 1991-03-14 Finnigan Mat Gmbh Verfahren und vorrichtung zur laserdesorption von analytmolekuelionen, insbesondere von biomolekuelen
RU2124783C1 (ru) * 1994-06-07 1999-01-10 Александр Алексеевич Макаров Способ анализа макромолекул биополимеров
DE19617011A1 (de) * 1996-04-27 1997-11-06 Bruker Franzen Analytik Gmbh Verfahren zur matrixunterstützten ionisierenden Laserdesorption

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4006381A1 (fr) 2009-04-16 2022-06-01 Fallbrook Intellectual Property Company LLC Ensemble stator et mécanisme de changement de vitesse pour transmission variable en continu

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