CN106324073A - Two-dimension substrate aiming at surface assisted laser desorption ionization mass spectrometry - Google Patents
Two-dimension substrate aiming at surface assisted laser desorption ionization mass spectrometry Download PDFInfo
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- CN106324073A CN106324073A CN201610816062.9A CN201610816062A CN106324073A CN 106324073 A CN106324073 A CN 106324073A CN 201610816062 A CN201610816062 A CN 201610816062A CN 106324073 A CN106324073 A CN 106324073A
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- 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
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Abstract
The invention discloses a two-dimension substrate aiming at surface assisted laser desorption ionization mass spectrometry. The surface of the two-dimension substrate is divided into a plurality of areas, each area contains an array of a two-dimension microstructure (21), the arrangement mode of the areas is a rectangular array, and the two-dimension microstructures (21) in different areas are identical or different; a sample is directly loaded on the substrate, the two-dimension microstructures (21) on the surface of the substrate are coupled with laser and absorb and transfer laser energy to to-be-tested analyte molecules to enable the to-be-tested analyte molecules to desorb and to be cracked into charged molecular fragments. The sample is directly loaded on the substrate, the two-dimension microstructures on the surface of the substrate are coupled with the laser and absorb and transfer the laser energy to the to-be-tested analyte molecules to enable the to-be-tested analyte molecules to desorb and to be cracked into the charged molecular fragments.
Description
Technical field
The invention belongs to exempt from substrate mass spectral analysis field, (surface assisted laser solution is sucked away from towards SALDI to be specifically related to a class
Sonization) substrate of mass spectrographic two dimension.
Background technology
Substance assistant laser desorpted ionizing (Matrix-Assisted Laser Desorption/Ionization,
MALDI) since invention, it is widely used in the biomacromolecule such as polypeptide, albumen and cell, the Analysis and Identification of tissue, once obtains 2002
Year Nobel chemistry Prize.But the substrate in MALDI is harsher to sample salinity, and the analyte signal to low charge-mass ratio district
There is severe jamming.Therefore, exploitation can match in excellence or beauty MALDI Ionization Efficiency to exempt from matrix base significant, it sets substantially
Meter thinking is that the microstructure utilizing substrate surface couples with laser and absorbs part luminous energy, then transfers to sample molecule
Help its desorbing and ionizing, referred to as surface assisted laser desorption ionization (Surface Assisted Laser
Desorption/Ionization, SALDI).
SALDI substrate at present can be divided mainly into carbon-based material (graphite granule, fullerene, CNT etc.), nano-particle
Material (germanium, gold, silver, platinum, silicon, tungsten oxide, titanium dioxide etc.) and grade micro-surface structure (the sub-micro rice noodle of porous silicon, silicon or aluminum,
Post, well etc.).Hypothesis for laser desorption ionization (LDI) process includes induced with laser pyrolysis absorption (Laser Induced
Thermal Desorption), laser induced surface melt (Laser Induced Surface Melting), interior can convert
(Internal Energy Transfer), gas expansion explosion (Gas Expansion) etc..California, USA university Wei J. and
First partner reports silica-based desorption ionization technique, the porous silicon that they obtain with electrochemical corrosion silicon chip on Nature
Instead of the substrate target in MALDI, demonstrate the DIOS each quasi-molecule for 150-12000Da, and saturated salt solution eases up
Rush liquid can effectively detect.Jilin University Lv Nan teaches seminar and utilizes optical etching technology to be prepared for orderly silicon nanorods battle array
Row, experiment finds that laser light absorbing efficiency is correlated with substrate micro structure, increases specific surface area and can promote absorbance, but energy dissipation is also
Strengthen therewith.Germany Kraus T. and partner are prepared for orderly submicron silicon pore array and are used as SALDI substrate, find that it is carried on the back
Scape noise is relatively low.From different aspects, these results of study confirm that micro structure the most actively improves light suction with being coupled with of laser
Receipts, transformation efficiency.
The present invention relates to the class two-dimentional substrate towards SALDI, utilize laser local effect in two dimension micro structure
Strengthen the substrate analyzing efficiency to sample.
Summary of the invention
Technical problem: the present invention is the class two-dimentional substrate towards surface assisted laser desorption ionization mass spectra, above-mentioned two
Detectable analyte at the bottom of Wiki is generally nucleic acid, nucleotide, polypeptide, protein, saccharide, lipid, synthetic polymer, metabolism product
Thing, medicine, environmental water sample, soil extract thing etc..
Technical scheme: the present invention is the class two-dimentional substrate towards surface assisted laser desorption ionization mass spectra, this two dimension
Substrate surface is divided into some regions, each region to comprise the array of two dimension micro structure, and its arrangement mode is rectangular array, not same district
Two-dimentional micro structure in territory is identical or different；The direct appendix of sample in substrate, the two-dimentional micro structure of substrate surface and laser coupled,
Absorb and shift laser energy to test analyte molecule, be allowed to desorption and be cracked into charged molecular fragment.
Monocrystal silicon is selected in described two-dimentional substrate, and resistivity is 0.001～100 Ω cm.
Described two-dimentional microstructure size is 50nm～20 μm, and it is most advanced and sophisticated or slit separation is 20～100nm.
Described two-dimentional micro structure, one or more in its surface evaporation silver, gold, platinum, palladium, copper, thickness be 10～
100nm。
Described laser is ps pulsed laser and ns pulsed laser, pulse energy peaks 0.01～100mJ, pulsewidth 1～10ns, frequency 1～
100Hz, wavelength concentrates on ultra-violet (UV) band or near infrared region.
Beneficial effect: for above-mentioned two dimension substrate laser be ps pulsed laser and ns pulsed laser, pulse energy peaks 0.01～
100mJ, pulsewidth 1～10ns, frequency 1～100Hz, wavelength concentrate on ultra-violet (UV) band (such as 337nm, 355nm) or near infrared region (as
1064nm)。
The above-mentioned two dimension detectable analyte of substrate is generally nucleic acid, nucleotide, polypeptide, protein, saccharide, lipid, conjunction
Become polymer, metabolite, medicine, environmental water sample, soil extract thing etc..
The present invention does not use substrate, and the direct appendix of sample, in substrate, the two-dimentional micro structure of substrate surface and laser coupled, is inhaled
Receive and shift laser energy to test analyte molecule, be allowed to desorption and be cracked into charged molecular fragment.
Accompanying drawing explanation
The invention will be further described with embodiment below in conjunction with the accompanying drawings:
Fig. 1 is the present invention towards SALDI mass spectrographic two dimension substrate, wherein has monocrystalline silicon-based bulk 11, the one of substrate surface
Individual region 12, the Two Areas 13 of substrate surface.
Fig. 2 is the array of the two-dimentional micro structure of Two Areas 13 correspondence in Fig. 1, wherein has two-dimentional micro structure 21, single
Brilliant silicon-based bulk 22.
Fig. 3 is the two-dimentional microstructure unit 21 of in Fig. 2, wherein has the micro structure main body 31 protruding plane, monocrystal silicon
Base plane 32, two close most advanced and sophisticated hot spot regions 33 formed.
Fig. 4 is 4 most advanced and sophisticated two dimension microstructure units.
Fig. 5 is 8 most advanced and sophisticated two dimension microstructure units.
Fig. 6 is 16 tips/slit two dimension microstructure unit.
Fig. 7 is that unicuspid splits two dimension microstructure unit.
Fig. 8 is single wedge two dimension microstructure unit.
Fig. 9 is single slit two-dimensional structure unit.
Figure 10 is half-blindness list slit two-dimensional structure unit.
Figure 11 is T-shaped slit two-dimensional structure unit.
Figure 12 is cross slits two-dimensional structure unit.
Figure 13 is double circle slit two-dimensional structure unit.
Detailed description of the invention
The present invention is a class towards SALDI mass spectrographic two dimension substrate, and this two dimension substrate surface is divided into some regions, Mei Gequ
Territory comprises the array of two dimension micro structure, and its arrangement mode is rectangular array, and the two-dimentional micro structure in zones of different is identical or different；
The direct appendix of sample, in substrate, the two-dimentional micro structure of substrate surface and laser coupled, absorbs and shifts laser energy to be measured point
Analysis thing molecule, is allowed to desorption and is cracked into charged molecular fragment.
Monocrystal silicon is selected in described two-dimentional substrate, and resistivity is 0.001～100 Ω cm.
Described two-dimentional microstructure size is 50nm～20 μm, and it is most advanced and sophisticated or slit separation is 20～100nm, uses and focuses on
Ion beam or electron beam lithography processing.
Described two-dimentional micro structure, one or more in its surface evaporation silver, gold, platinum, palladium, copper, thickness be 10～
100nm。
Described laser is ps pulsed laser and ns pulsed laser, pulse energy peaks 0.01～100mJ, pulsewidth 1～10ns, 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, nucleotide, polypeptide, protein, saccharide, lipid, synthetic polymer, metabolism product
Thing, medicine, environmental water sample, soil extract thing etc..
Further illustrate below in conjunction with specific embodiment.Should be understood that this embodiment is for illustrating that the present invention is not limited to
Limit the scope of the present invention.The implementation condition used in embodiment can be entered shape according to practical situation and adjust.
Embodiment 1 exempts from substrate two dimensional surface substrate food additive detection in beverage
Fig. 2 very diagrammatically show a kind of double most advanced and sophisticated micro structure array substrate, and wherein two dimension micro structure 21 uses double most advanced and sophisticated micro-
Construction unit, is two isosceles right triangles utilizing focused-ion-beam lithography to obtain, a length of 500nm of hypotenuse, its surface
Being deposited with the titanium of 10nm and the gold of 40nm respectively, two most advanced and sophisticated spacing are 30nm.By supermarket buy mineral water, soda pop, red wine,
After the beverage extractings such as milk product concentrate, drip after taking 10 μ L respectively on the double most advanced and sophisticated micro structure array of two dimension substrate, naturally dry in the air
Dry.Selecting the nanosecond laser of 355nm, its peak value of pulse energy is 50 μ J, pulsewidth 3ns, frequency 10Hz.Select normal pressure open type
Input mode, utilizes quadrupole rod mass spectrometer, and the time of integration, 50ms, followed the tracks of conventional food additive, and melamine respectively
The illegal additive content in all kinds of beverages such as amine, tonyred.
Embodiment 2 exempts from substrate two dimensional surface substrate for biological detection
Fig. 4 very diagrammatically show a kind of 4 most advanced and sophisticated two dimension microstructure units, and it utilizes 4 that focused-ion-beam lithography obtains
Isosceles right triangle, a length of 500nm of hypotenuse, its surface is deposited with the titanium of 10nm and the gold of 40nm respectively, between two most advanced and sophisticated
Away from for 30nm.Sample in the present embodiment loads and experiment condition is similar with embodiment 1.
For simplifying statement, every kind of two-dimentional microstructure unit corresponding in Fig. 5 to Figure 13, all use similar with the present embodiment
Technique be prepared, sample load and testing conditions similar with the present embodiment 1.
Claims (5)
1. a class is towards the two-dimentional substrate of surface assisted laser desorption ionization mass spectra, it is characterised in that this two dimension substrate (11)
Surface is divided into some regions, each region (13) to comprise the array of two dimension micro structure (21), and its arrangement mode is rectangular array, no
Identical or different with the two-dimentional micro structure (21) in region；The direct appendix of sample is in substrate, the two-dimentional micro structure of substrate surface
(21) and laser coupled, absorb and shift laser energy to test analyte molecule, be allowed to desorption and be cracked into charged point
Sub-fragment.
A class the most according to claim 1 is towards the two-dimentional substrate of surface assisted laser desorption ionization mass spectra, its feature
Being, monocrystal silicon is selected in described two-dimentional substrate (11), and resistivity is 0.001～100 Ω cm.
A class the most according to claim 1 is towards the two-dimentional substrate of surface assisted laser desorption ionization mass spectra, its feature
Being, described two-dimentional micro structure (21) a size of 50nm～20 μm, it is most advanced and sophisticated or slit separation is 20～100nm.
The most according to claim 3, a class exists towards the two-dimentional substrate of surface assisted laser desorption ionization mass spectra, its feature
In, described two-dimentional micro structure (21), one or more in its surface evaporation silver, gold, platinum, palladium, copper, thickness be 10～
100nm。
A class the most according to claim 1 is towards the two-dimentional substrate of surface assisted laser desorption ionization mass spectra, its feature
Being, described laser is ps pulsed laser and ns pulsed laser, pulse energy peaks 0.01～100mJ, pulsewidth 1～10ns, frequency 1～
100Hz, wavelength concentrates on ultra-violet (UV) band or near infrared region.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107014891A (en) * | 2017-01-24 | 2017-08-04 | 东南大学 | A kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra |
| 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 |
| CN114887862A (en) * | 2022-05-10 | 2022-08-12 | 华南农业大学 | nanoparticle-hPDA-TDNT material and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107014891A (en) * | 2017-01-24 | 2017-08-04 | 东南大学 | A kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra |
| CN107014891B (en) * | 2017-01-24 | 2019-11-08 | 东南大学 | A kind of spiral tetrahexahedron structural substrates for laser desorption ionization mass spectra |
| 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 |
| CN114887862A (en) * | 2022-05-10 | 2022-08-12 | 华南农业大学 | nanoparticle-hPDA-TDNT material and preparation method and application thereof |
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Application publication date: 20170111 |