CN107014891A - A kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra - Google Patents
A kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra Download PDFInfo
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- CN107014891A CN107014891A CN201710054015.XA CN201710054015A CN107014891A CN 107014891 A CN107014891 A CN 107014891A CN 201710054015 A CN201710054015 A CN 201710054015A CN 107014891 A CN107014891 A CN 107014891A
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- spiral tetrahexahedron
- tetrahexahedron
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- spiral
- desorption ionization
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
Abstract
The invention discloses a kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra, the substrate is three-dimensional network-like structure, surface covers one layer of noble metal, it can be coupled with laser, absorb and shift laser energy to test analyte molecule, be allowed to be desorbed and be cracked into electrically charged molecular fragment.Described spiral tetrahexahedron structure (Gyroid structures) obeys following relation：Wherein L is the cycle of spiral tetrahexahedron structure, and t adjusts the pattern of spiral tetrahexahedron structure.
Description
Technical field
The invention belongs to exempt from matrix mass spectral analysis field, and in particular to a kind of for laser desorption ionization mass spectra
Spiral tetrahexahedron structural substrates.
Background technology
Laser desorption ionization (Laser Desorption/Ionization, LDI) is one kind weight in mass spectral analysis field
" soft ionization " technology wanted, is mainly used in large biological molecule (such as polypeptide, albumen) and cell, tissue and analyzes and identifies, matrix
Laser desorption ionization (MALDI) technology of auxiliary once obtained Nobel chemistry Prize in 2002.Matrix is a double-edged sword, although easily
Change LDI processes, but easily influenceed by salt content in sample, and have severe jamming to the analyte signal in low charge-mass ratio area.Cause
This, exempts from matrix base significant for laser desorption ionization mass spectra.Its Basic Design thinking is to utilize substrate surface
Microstructure coupled with laser and absorb part luminous energy, then transfer to sample molecule help its desorb and ionize,
Referred to as surface assisted laser desorption ionization (Surface Assisted Laser Desorption/Ionization, surface
Assisted laser desorption is ionized).
Current surface assisted laser desorption ionization substrate can be divided mainly into carbon-based material, and (graphite particle, fullerene, carbon are received
Mitron etc.), nano-particle material (germanium, gold, silver, platinum, silicon, tungsten oxide, titanium dioxide etc.) and grade micro-surface structure (porous silicon, silicon
Or sub-micro rice noodles, post, the well of aluminium etc.).Jilin University Lv Nan professors seminar is prepared for orderly silicon using optical etching technology and received
Rice cone array, experiment finds that laser light absorbing efficiency is related with substrate micro-structural, and increase specific surface area can lift absorptivity, but energy
Dissipation also strengthens therewith.California, USA university Wei J. and partner report silicon substrate desorption ionization technique on Nature,
The porous silicon that they are obtained with electrochemical corrosion silicon chip instead of the matrix target in MALDI, demonstrate DIOS for 150-
12000Da each quasi-molecule, and saturated salt solution and buffer solution can effective detections.These results of study are demonstrate,proved from different aspects
Real micro-structural and laser are coupled with beneficial to actively improving light absorbs, transformation efficiency.
The content of the invention
Technical problem：It is an object of the invention to provide a kind of spiral tetrahexahedron for laser desorption ionization mass spectra
Structural substrates, are related to a kind of three-dimensional substrates towards surface assisted laser desorption ionization, using laser at the four sides of spiral 20
Local effect in body three-dimensional microstructures strengthens desorption efficiency of the substrate to sample.
Technical scheme：The present invention is a kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra,
The substrate is three-dimensional network-like structure, and surface covers one layer of noble metal, can be coupled with laser, absorb and shift laser energy
To test analyte molecule, it is allowed to be desorbed and is cracked into electrically charged molecular fragment.
Described spiral tetrahexahedron structure obeys below equation：
Wherein L is the cycle of spiral tetrahexahedron structure, and t adjusts the pattern of spiral tetrahexahedron structure.
Described spiral tetrahexahedron structure, its skeleton is printed by two-photon and prepared, and the noble metal of surface covering leads to
Cross the acquisition of the approach such as electroless plating, ald, electron beam evaporation.
Described spiral tetrahexahedron structural framework, its cycle is 0.5~50 μm, a diameter of 0.1~1 μm of bone beam, bone
Frame material is that framework material is thick film photolithography glue (SU8), dimethyl silicone polymer (PDMS) or polyethyleneglycol diacrylate
(PEGDA) photoresist of the group containing acrylamide.
The noble metal of described spiral tetrahexahedron body structure surface is silver, gold, platinum, palladium or titanium, thickness for 10~
500nm。
Described laser be ps pulsed laser and ns pulsed laser, 0.01~100mJ of pulse energy peaks, 1~10ns of pulsewidth, frequency 1~
100Hz, wavelength concentrates on ultra-violet (UV) band (such as 337nm, 355nm) or near infrared region (such as 1064nm).
Described analyte is generally nucleic acid, nucleotides, polypeptide, protein, carbohydrate, lipid, synthetic polymer, metabolism production
Thing, medicine, environmental water sample or soil extract thing.
Beneficial effect：There is spiral tetrahexahedron structure prepared by two-photon printing relatively low volume fraction (can be less than
5%), so as to larger specific surface area, can fully be contacted in determinand, detection sensitivity is improved.Meanwhile, spiral 20
Tetrahedral structure belongs to photon crystal material, can occur strong interaction with the laser of certain wavelength, so as to be measured
The light absorption process and ionization process of thing are all strengthened.
Brief description of the drawings
The invention will be further described with reference to the accompanying drawings and examples：
Fig. 1 is that a kind of work of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra of the invention is former
Reason, wherein having：The three-dimensional mass spectrum substrate 11 of spiral tetrahexahedron structure, spiral tetrahexahedron micro-structural 12, thing to be detected
13, nanosecond laser beam 14, the electrically charged molecular fragment 15 parsed.
Fig. 2 is 27 spiral tetrahexahedron construction units, corresponding to t=0.4.
Fig. 3 is 27 spiral tetrahexahedron construction units, corresponding to t=1.1.
Fig. 4 is 27 spiral tetrahexahedron construction units, corresponding to t=1.4.
Fig. 5 is the single spiral tetrahexahedron construction unit printed for two-photon, corresponding to L=10 μm, t=
1.15.
Fig. 6 is the schematic perspective view that two-photon prints spiral tetrahexahedron structure.
Fig. 7 is the electron scanning micrograph of spiral tetrahexahedron structural framework.
Embodiment
Further illustrated below in conjunction with specific embodiment.It should be understood that the embodiment is to be used to illustrate the present invention and be not limited to
Limit the scope of the present invention.The implementation condition used in embodiment can enter shape adjustment according to practical situation.
The present invention is a kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra, and the substrate is three
Network-like structure is tieed up, surface covers one layer of noble metal, can be coupled with laser, absorb and shift laser energy to analysis to be measured
Thing molecule, is allowed to be desorbed and is cracked into electrically charged molecular fragment.
Described spiral tetrahexahedron structure obeys below equation：
Wherein L is the cycle of spiral tetrahexahedron structure, and t adjusts the pattern of spiral tetrahexahedron structure.
Surface assisted laser desorption ionization substrate of the embodiment 1 based on spiral tetrahexahedron structure is exploded for trace
The detection of thing
Fig. 1 very diagrammatically show the three-dimensional substrates based on spiral tetrahexahedron structure and is sucked away from for surface assisted laser solution
The operation principle of sonization detection.Wherein the main body 11 of substrate, is typically chosen highly doped monocrystalline silicon, and its resistivity is 0.01~100
Ω cm, thickness is 525 μm；The spiral tetrahexahedron structural framework 12 of two-photon printing, structural cycle L is 1 μm, processing essence
It is 200nm to spend (bone beam diameter), and the colloid gold particle of one layer of 100nm thickness is adsorbed on skeleton surface using non-electrolytic plating method.Spiral shell
Revolve tetrahexahedron structure to be heat-treated 5 minutes through 150 DEG C under atmosphere of inert gases, naturally cool to room temperature.Containing thing to be detected
Sample be dissolved in atent solvent, take 20 μ L to be added drop-wise to spiral tetrahexahedron surface, dry naturally.From receiving for 355nm
Second laser, its peak value of pulse energy is 50 μ J, pulsewidth 3ns, frequency 10Hz.From normal pressure open type input mode, four are utilized
Pole bar mass spectrometer, time of integration 50ms.Observation treats whether contain explosive and its content in test sample.
Claims (7)
1. a kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra, it is characterised in that the substrate is
Three-dimensional network-like structure, surface covers one layer of noble metal, can be coupled with laser, absorb and shift laser energy to be measured point
Thing molecule is analysed, is allowed to be desorbed and is cracked into electrically charged molecular fragment.
2. a kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra according to claim 1 its
It is characterised by, described spiral tetrahexahedron structure obeys following relation：
Wherein L is the cycle of spiral tetrahexahedron structure, and t adjusts the pattern of spiral tetrahexahedron structure.
3. a kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra according to claim 1,
It is characterized in that described spiral tetrahexahedron structure, its skeleton is printed by two-photon and prepared, the noble metal of surface covering
Obtained by approach such as electroless plating, ald, electron beam evaporations.
4. a kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra according to claim 3,
It is characterized in that described spiral tetrahexahedron structural framework, its cycle is 0.5~50 μm, a diameter of 0.1~1 μm of bone beam,
Framework material is that thick film photolithography glue SU8, polydimethylsiloxane or polyethyleneglycol diacrylate PEGDA contain acrylamide
The photoresist of group.
5. a kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra according to claim 3,
It is characterized in that the noble metal of described spiral tetrahexahedron body structure surface is silver, gold, platinum, palladium or titanium, thickness for 10~
500nm。
6. a kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra according to claim 1,
It is characterized in that described laser is ps pulsed laser and ns pulsed laser, 0.01~100mJ of pulse energy peaks, 1~10ns of pulsewidth, frequency 1
~100Hz, wavelength concentrates on ultra-violet (UV) band or near infrared region.
7. a kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra according to claim 1,
It is characterized in that described analyte is nucleic acid, nucleotides, polypeptide, protein, carbohydrate, lipid, synthetic polymer, metabolism production
Thing, medicine, environmental water sample or soil extract thing.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107966491A (en) * | 2017-11-17 | 2018-04-27 | 南京大学 | A kind of surface assisted laser desorption ionization mass spectra substrate based on porous membrane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101329301A (en) * | 2007-06-19 | 2008-12-24 | 佳能株式会社 | Substrate for mass spectrometry, mass spectrometry, and mass spectrometer |
| CN106324073A (en) * | 2016-09-12 | 2017-01-11 | 东南大学 | Two-dimension substrate aiming at surface assisted laser desorption ionization mass spectrometry |
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- 2017-01-24 CN CN201710054015.XA patent/CN107014891B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101329301A (en) * | 2007-06-19 | 2008-12-24 | 佳能株式会社 | Substrate for mass spectrometry, mass spectrometry, and mass spectrometer |
| CN106324073A (en) * | 2016-09-12 | 2017-01-11 | 东南大学 | Two-dimension substrate aiming at surface assisted laser desorption ionization mass spectrometry |
Non-Patent Citations (1)
| Title |
|---|
| MASAYUKI ADACHI等: "Incorporation of Metal Nanoparticles into a Double Gyroid Network Texture", 《MACROMOLECULES》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107966491A (en) * | 2017-11-17 | 2018-04-27 | 南京大学 | A kind of surface assisted laser desorption ionization mass spectra substrate based on porous membrane |
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