CN109119323A - Multichannel mass spectrum nozzle needle and preparation method thereof based on macropore perfusion microballoon - Google Patents
Multichannel mass spectrum nozzle needle and preparation method thereof based on macropore perfusion microballoon Download PDFInfo
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- CN109119323A CN109119323A CN201810782412.3A CN201810782412A CN109119323A CN 109119323 A CN109119323 A CN 109119323A CN 201810782412 A CN201810782412 A CN 201810782412A CN 109119323 A CN109119323 A CN 109119323A
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- nozzle needle
- perfusion
- microballoon
- macropore
- mass spectrum
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- 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
- H01J49/165—Electrospray ionisation
- H01J49/167—Capillaries and nozzles specially adapted therefor
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
Multichannel mass spectrum nozzle needle and preparation method thereof based on macropore perfusion microballoon, is related to multichannel mass spectrum nozzle needle.Multichannel mass spectrum nozzle needle based on macropore perfusion microballoon is equipped with mass spectrum nozzle needle and macropore perfusion microballoon, and the diameter of the macropore perfusion microballoon is identical as the internal diameter of mass spectrum nozzle needle, and the macropore perfusion microballoon is fixed on the spout of mass spectrum nozzle needle.By the polyamide coating layer of quartz capillary burning-off one end, 1cm long quartz capillary is exposed, polishes, obtains the mass spectrum nozzle needle of certain taper；The perfusion silicon ball that one outer diameter is 75 μm is put into one end of quartz capillary, and silicon ball is pushed into nozzle using capillary, silicon ball is fixed in nozzle, obtains the multichannel mass spectrum nozzle needle based on macropore perfusion microballoon.The nozzle needle of preparation will not generate change to the original shape of nozzle needle and application method, not influence the normal use of nozzle needle, versatile.
Description
Technical field
The present invention relates to multichannel mass spectrum nozzle needle, more particularly, to it is quick and easy with preparation method, do not influence outside nozzle needle
Shape and the series of advantages such as application method, versatile can be applied to filling based on macropore for all electrospray ionization mass spectrum detectors
Flow the multichannel mass spectrum nozzle needle and preparation method thereof of microballoon.
Background technique
Mass spectrum is most widely used at present, qualitatively and quantitatively one of highest detection technique of detection sensitivity, in mass spectrum
Ion source category has very much, and electric spray ion source is widely applied by its unique advantage.In order to improve electron spray
The efficiency of ion source, many researchers are optimized and develop to the design of nozzle needle, and wherein multichannel nozzle needle technology is
Important research direction.Using the spraying method of multichannel, the liquid with high surface area/volume ratio smaller size can produce
Drop, the concentration for increasing droplet surface analyte, can fast implement desolvation process, improve Ionization Efficiency, reduce solvent
Effect and ion depression effect.Current research mainly has: by being sprayed to form multiple channels by more nozzle needle parallel exhausts
Mouthful (Cox J.T., et al., J.Am.Soc.Mass Spectr., 2014,25,2028；Su S.,et al.,
Anal.Chem.,2009,81,7281)；Using advanced manufacturing technology, multiple flow path channels are produced in single nozzle needle, thus
Realize that multichannel is spraying (Gibson G.T., et al., J.Mass Spectr., 2012,47,271)；There are also utilize integral post
Technology, formed in nozzle needle multi-channel flow passage (Koerner T., et al., Anal.Chem., 2004,76,6456；Koerner
T.,et al.,Anal.Chem.,2007,79,3312；Bedair M.F.,et al.,Anal.Chem.,2006,78,
1130).In the design of the above multichannel nozzle needle, preparation method is complicated, the multichannel Limited Number of formation, and needs to confront
Spectrometer, which carries out corresponding improve, to be used, and universality is poor.
Summary of the invention
The object of the present invention is to provide it is quick and easy with preparation method, do not influence nozzle needle shape and application method, general
Property the series of advantages such as strong, can be applied to the multichannel mass spectrum based on macropore perfusion microballoon of all electrospray ionization mass spectrum detectors
Nozzle needle and preparation method thereof.
The multichannel mass spectrum nozzle needle based on macropore perfusion microballoon is equipped with mass spectrum nozzle needle and macropore perfusion microballoon, described big
The diameter of hole perfusion microballoon is identical as the internal diameter of mass spectrum nozzle needle, and macropore perfusion microballoon is fixed on the spout of mass spectrum nozzle needle.
Common nozzle needle can be used in the mass spectrum nozzle needle.
The common nozzle needle refers to the nozzle needle that can be applied to electric spray ion source mass detector, common nozzle needle include but
It is not limited to constant inner diameter nozzle needle, internal diameter gradual change nozzle needle, taper nozzle needle etc..
The common nozzle needle can be the big flow for high performance liquid chromatography/ultra performance liquid chromatography (HPLC/UHPLC)
Nozzle needle, be also possible to for receive stream liquid chromatogram receive stream nozzle needle.
The internal diameter of the common nozzle needle can be 5~500 μm.
Inorganic material or organic polymer material can be used in the material of the common nozzle needle, and the inorganic material can be selected from stone
Polyether-ether-ketone (PEEK) etc. can be used in one of English, metal etc., the organic polymer material.
A large amount of ducts are run through in the inside of the macropore perfusion microballoon, spraying for realizing multichannel.
The macropore perfusion microballoon has through hole abundant, and permeability is strong, very small to flowing phase resistance power.
The material of the macropore perfusion microballoon can be selected from silica inorganic material, organic polymer material, organic-inorganic
It is a kind of in hybrid material etc..
The method that the macropore perfusion microballoon is fixed on nozzle needle nozzle can be based on foundation stone effect (Key Stone
Effect), the physical methods such as thermal deformation mechanical presses are also possible to bind using chemical reaction method in nozzle.
The macropore perfusion microballoon can be put into nozzle needle from nozzle needle mobile phase spout end or nozzle needle mobile phase arrival end.
When the macropore perfusion microballoon is put into from nozzle needle mobile phase arrival end, microballoon first can be placed on arrival end, then
It is less than the capillary of nozzle needle internal diameter with outer diameter or wire pushes to nozzle.
The preparation method of the multichannel mass spectrum nozzle needle based on macropore perfusion microballoon the following steps are included:
1) by the polyamide coating layer of quartz capillary burning-off one end, quartz capillary is exposed, polishes, obtains certain taper
Mass spectrum nozzle needle；
In step 1), the internal diameter of the quartz capillary can be 75 μm, and the length of quartz capillary can be 4cm；It is described
The length for exposing quartz capillary can be 1cm；The polishing can be used fine sandpaper and polish in capillary one end.
2) perfusion silicon ball is put into one end of quartz capillary, and silicon ball is pushed into capillary spout using capillary
Place, is fixed on capillary nozzle for perfusion silicon ball, obtains the multichannel mass spectrum nozzle needle based on macropore perfusion microballoon.
In step 2), the outer diameter of the perfusion silicon ball can be 75 μm；The outer diameter of the capillary can be 50 μm.
The nozzle needle prepared in the present invention will not generate change to the original shape of nozzle needle and application method, not influence nozzle needle
Normal use, it is versatile.
The shortcomings that in order to overcome existing multichannel mass spectrum nozzle needle, nozzle needle provided by the invention are based on macropore perfusion microsphere-rich
It is spraying to realize multichannel for uniform through hole.Only macropore perfusion microballoon need to be placed and secured in nozzle needle spout when preparation
Place.This nozzle needle contains a large amount of micro/nano-scale spray channel, can greatly improve spray effect；And preparation method is simple,
Universality is strong, and producing efficiency is high, favorable reproducibility, has huge application prospect.
Detailed description of the invention
Fig. 1 is the preparation process schematic diagram of mass spectrum nozzle needle embodiment of the present invention.
Fig. 2 is foundation stone effect schematic diagram of the present invention.
Fig. 3 is commercialization nozzle needle multichannelization front and back mass ions signal contrast figure in embodiment 3.In Fig. 3, curve a
For mass ions signal after nozzle needle multichannel, curve b is commercialization nozzle needle mass ions signal
Fig. 4 is Hela cell protein group analysis of spectra in embodiment 4.
Specific embodiment
The invention will be further described with several alternative embodiments with reference to the accompanying drawing.Specific skill is not specified in embodiment
Art and condition person carry out according to technology described in document in the art and condition or according to product description, agents useful for same or
Production firm person is not specified in instrument, and being can be by commercially available obtained conventional products.
Embodiment 1: internal diameter is the preparation of 75 μm of multichannel quartz nozzle needles
As shown in Figure 1, the quartz capillary 4cm that interception internal diameter is 75 μm, exposed with flame burning-off one end polyamide coating layer
1cm long quartz capillary 1 out is polished long 1 one end of quartz capillary using fine sandpaper, obtains the mass spectrum spray of certain taper
Needle.The perfusion silicon ball 2 that one outer diameter is 75 μm is put into the other end, and is pushed silicon ball using the capillary 3 that outer diameter is 50 μm
To nozzle, due to foundation stone effect (Key Stone Effect) (Fig. 2), silicon ball is fixed in nozzle, by pressure test,
Silicon ball can withstand up to the pressure of 6000psi (40MPa).
Embodiment 2: application of the novel multi-channel nozzle needle in mass spectrum
By the multichannel mass spectrum nozzle needle prepared in embodiment 1 be integrated into Waters ACQUITY Nano-UPLC (Waters,
Milford, MA, USA) in/Q-Exactive mass spectrograph (Thermo Scientific, USA) combined system, and realize good
It is spraying.
Embodiment 3: multichannel is carried out to commercialization nozzle needle using macropore perfusion microballoon
Commercialization mass spectrum nozzle needle (ThermoScientific, ES542,150 μm of OD, 30 μm of ID) is taken, embodiment 1 is utilized
In method, be that 30 μm of perfusion silicon ball places and is fixed on nozzle by an internal diameter.Utilize Hela cell polypeptide enzymolysis liquid
To the nebulization efficiency of mass spectrum nozzle needle before and after multichannelization, i.e. Mass Spectrometer Method ion peak intensity carries out characterization comparison.As a result such as Fig. 3 institute
Show, after multichannel, the nebulization efficiency of nozzle needle is significantly improved, and Mass Spectrometer Method ionic strength is obviously improved.
Embodiment 4: multichannel is carried out to commercialization nozzle needle using macropore perfusion microballoon
Using nozzle needle prepared in embodiment 3, based on Waters ACQUITY Nano-UPLC (Waters,
Milford, MA, USA)/Q-Exactive mass spectrograph (Thermo Scientific, USA) combination proteomics platform, it is right
Hela cell polypeptide enzymolysis liquid carries out proteome analysis, and gained proteomics spectrogram is as shown in figure 4, utilize Thermo
The 1.4 proteomics data processing platform of Proteome Discoverer of Fisher company is to gained proteomics data
Protein identification is carried out, identifying polypeptide number is 9321, protein number 3239.
The present invention is combined and is prepared by common nozzle needle and macropore perfusion microballoon: it is based on foundation stone effect, macropore perfusion is micro-
Ball is fixed on nozzle needle nozzle；Since macropore perfusion microballoon has abundant and uniform hole, the diameter macropores of surface perforation are
1000nm or so, therefore it is spraying to form multichannel liquid stream.This novel nozzle needle preparation method is simple, and gained nozzle needle is versatile；
The substantial increase of spout quantity is capable of forming more smaller taylor cones, to generate the micro-nano drop with bigger serface；
Drop size reduces the concentration that will increase droplet surface analyte, and can faster realize desolvation process, then can
Ionization Efficiency is significantly improved, solvent effect and ion depression effect are reduced, reduces the generation of nozzle needle stopping state；It is new using this
It is higher, more stable can to make detected signal value for type nozzle needle, and is able to extend nozzle needle service life.
Claims (10)
1. the multichannel mass spectrum nozzle needle based on macropore perfusion microballoon, it is characterised in that it is equipped with mass spectrum nozzle needle and macropore perfusion microballoon,
The diameter of the macropore perfusion microballoon is identical as the internal diameter of mass spectrum nozzle needle, and the macropore perfusion microballoon is fixed on the spray of mass spectrum nozzle needle
Mouthful.
2. as described in claim 1 based on the multichannel mass spectrum nozzle needle of macropore perfusion microballoon, it is characterised in that the mass spectrum nozzle needle
Using common nozzle needle, the common nozzle needle refers to that the nozzle needle applied to electric spray ion source mass detector, common nozzle needle include
But it is not limited to constant inner diameter nozzle needle, internal diameter gradual change nozzle needle, taper nozzle needle.
3. as claimed in claim 2 based on the multichannel mass spectrum nozzle needle of macropore perfusion microballoon, it is characterised in that the common nozzle needle
Nozzle needle is flowed for high performance liquid chromatography/ultra performance liquid chromatography big flow nozzle needle or receiving for stream liquid chromatogram of receiving.
4. as claimed in claim 2 based on the multichannel mass spectrum nozzle needle of macropore perfusion microballoon, it is characterised in that the common nozzle needle
Internal diameter be 5~500 μm.
5. as claimed in claim 2 based on the multichannel mass spectrum nozzle needle of macropore perfusion microballoon, it is characterised in that the common nozzle needle
Material use inorganic material or organic polymer material, the inorganic material is selected from quartz, one of metal, described organic
Polymer material uses polyether-ether-ketone.
6. as described in claim 1 based on the multichannel mass spectrum nozzle needle of macropore perfusion microballoon, it is characterised in that the macropore perfusion
The material of microballoon is a kind of in silica inorganic material, organic polymer material, organic-inorganic hybrid material；The macropore
The method that perfusion microballoon is fixed on nozzle needle nozzle is based on foundation stone effect, thermal deformation mechanical presses physical method or to utilize chemistry
Reaction method is binded in nozzle.
7. as described in claim 1 based on the multichannel mass spectrum nozzle needle of macropore perfusion microballoon, it is characterised in that the macropore perfusion
Microballoon is put into nozzle needle from nozzle needle mobile phase spout end or nozzle needle mobile phase arrival end；The macropore perfusion microballoon is from nozzle needle mobile phase
It is that microballoon is first placed on arrival end when arrival end is put into, is then less than the capillary of nozzle needle internal diameter with outer diameter or wire pushes away
It send to nozzle.
8. the preparation method of the multichannel mass spectrum nozzle needle as described in claim 1~7 based on macropore perfusion microballoon, it is characterised in that
The following steps are included:
1) by the polyamide coating layer of quartz capillary burning-off one end, quartz capillary is exposed, polishes, obtains the matter of certain taper
Compose nozzle needle；
2) perfusion silicon ball is put into one end of quartz capillary, and silicon ball is pushed into capillary nozzle using capillary, it will
Perfusion silicon ball is fixed on capillary nozzle, obtains the multichannel mass spectrum nozzle needle based on macropore perfusion microballoon.
9. the preparation method of the multichannel mass spectrum nozzle needle based on macropore perfusion microballoon as claimed in claim 8, it is characterised in that
In step 1), the internal diameter of the quartz capillary is 75 μm, and the length of quartz capillary is 4cm；It is described to expose quartzy capillary
The length of pipe is 1cm；The polishing is to be polished using fine sandpaper in capillary one end.
10. the preparation method of the multichannel mass spectrum nozzle needle based on macropore perfusion microballoon as claimed in claim 8, it is characterised in that
In step 2), the outer diameter of the perfusion silicon ball is 75 μm；The outer diameter of the capillary is 50 μm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810782412.3A CN109119323A (en) | 2018-07-17 | 2018-07-17 | Multichannel mass spectrum nozzle needle and preparation method thereof based on macropore perfusion microballoon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810782412.3A CN109119323A (en) | 2018-07-17 | 2018-07-17 | Multichannel mass spectrum nozzle needle and preparation method thereof based on macropore perfusion microballoon |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112863995A (en) * | 2021-01-17 | 2021-05-28 | 复旦大学 | Method for manufacturing nano-spray needle of electrospray ion source |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5975426A (en) * | 1998-05-14 | 1999-11-02 | Waters Investments Limited | Use of porous beads as a tip for nano-electrospray |
| WO2007092227A3 (en) * | 2006-02-02 | 2008-06-26 | Battelle Memorial Institute | Monolithic electrospray ionization emitters and methods of making same |
| CN105679638A (en) * | 2016-03-25 | 2016-06-15 | 中国科学院成都生物研究所 | Electrospray ionization device and method based on microsphere |
| CN209056460U (en) * | 2018-07-17 | 2019-07-02 | 晋江精纯科技有限公司 | A kind of multichannel mass spectrum nozzle needle based on macropore perfusion microballoon |
-
2018
- 2018-07-17 CN CN201810782412.3A patent/CN109119323A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5975426A (en) * | 1998-05-14 | 1999-11-02 | Waters Investments Limited | Use of porous beads as a tip for nano-electrospray |
| WO2007092227A3 (en) * | 2006-02-02 | 2008-06-26 | Battelle Memorial Institute | Monolithic electrospray ionization emitters and methods of making same |
| CN105679638A (en) * | 2016-03-25 | 2016-06-15 | 中国科学院成都生物研究所 | Electrospray ionization device and method based on microsphere |
| CN209056460U (en) * | 2018-07-17 | 2019-07-02 | 晋江精纯科技有限公司 | A kind of multichannel mass spectrum nozzle needle based on macropore perfusion microballoon |
Non-Patent Citations (1)
| Title |
|---|
| TERRY KOEMER ET AL.: "Microsphere Entrapped Emitters for Sample Preconcentration and Electrospray Ionization Mass Spectrometry", 《ANAL.CHEM》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112863995A (en) * | 2021-01-17 | 2021-05-28 | 复旦大学 | Method for manufacturing nano-spray needle of electrospray ion source |
| CN112863995B (en) * | 2021-01-17 | 2022-05-20 | 复旦大学 | Manufacturing method of nano-spray needle of electrospray ion source |
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