CN103033556A - Device and mass spectrometry for direct electrospray ionization of sample on microfluidic chip - Google Patents
Device and mass spectrometry for direct electrospray ionization of sample on microfluidic chip Download PDFInfo
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Abstract
The invention belongs to the technical field of microfluidic chips, and particularly relates to a device and a mass spectrometry for direct electrospray ionization of a sample on a microfluidic chip. The device at least comprises a three-dimensional operating platform for placing the microfluidic chip, an electrode for providing spray voltage, a pulsed high-voltage power supply, and a mass spectrum arranged beside an ionization device, wherein the electrode for providing the spray voltage is not directly contacted with liquid in the microfluidic chip. A spray needle is not required to be fabricated or connected on the microfluidic chip, or the original design of a chip microchannel is not required to be changed, and a solution sample in the chip microchannel can be directly ionized by utilizing charge and discharge processes of pulsed voltage, and then the mass spectrometry can be conducted. In addition, a high-voltage in the device is not directly contacted with a solution, and the original function of the microfluidic chip is not affected due to chemical reaction on the electrode. The device is simple and convenient to operate, and is suitable for direct ionization and the mass spectrometry of the sample on the microfluidic chip.
Description
Technical field
The invention belongs to the micro-fluidic chip technical field, be specifically related to a kind of device and mass spectrometric analysis method that can be used for the direct electron spray ionisation of sample on the micro-fluidic chip.
Background technology
Microfluidic chip analysis is as operating platform take chip, simultaneously take analytical chemistry as the basis, take micro electronmechanical process technology as support, take the microchannel network as architectural feature, target is the function whole laboratory, comprise that sampling, dilution, reagent adding, reaction, separation, detection etc. are integrated on the microchip, and can repeatedly use.The microfluidic chip analysis technology have liquid flow controlled, consume sample and the characteristics such as reagent is few, analysis speed is fast, it is analyzed when can carry out up to a hundred samples within a few minutes even shorter time, and pre-service that can the canbe used on line sample and the overall process of analysis.Because it in the great potential in the fields such as biology, chemistry, medical science, has developed into the new focus of the subject crossing researchs such as a biology, chemistry, medical science, fluid, electronics, material, machinery.Also be based on These characteristics, the Flow Control analysis chip is called as " chip lab " (lab-on-a-chip) in the U.S., is called as " little confluence analysis chip " (micrototal analytical systems) in Europe.
Nowadays, the research that the micro-fluidic chip technology is used for life science develops into the emphasis that analysis field develops already, and mass spectrum also extensively has been subject to scientist's welcome as a kind of detection means of sensitivity.Micro-fluidic chip and mass spectral:mass spectrographic coupling technique combine micro-fluidic chip and mass spectral:mass spectrographic advantage, become the focus of everybody research.Aspect micro-fluidic and mass spectral:mass spectrographic interface, there have been a lot of experts and scholars to attempt.The beginning people use and insert kapillary derivation analysis liquid in the apertures of chip, then pass through threeway, thereby adding that voltage and conventional electron spray nozzle needle are sprayed carries out Mass Spectrometer Method, this mode of operation is simple, if but what use is that to receive the nozzle needle spraying of upgrading flow velocity routine unstable, the signal that obtains is just very poor; The bright seminar of holding of the woods of the Dalian Chemistry and Physics Institute has improved this spray pattern, has used the sheath flow liquid body, make the spraying signal stabilization, but sheath flow liquid has diluted sample to a certain extent, has sacrificed mass spectral:mass spectrographic sensitivity; The Luo Guoan seminar of Tsing-Hua University, the processing porous membrane structure is realized current lead-through on micro-fluidic chip, as chip and mass spectral:mass spectrographic interface, but job sequence is complicated, also is difficult for spread; In recent years, there was successively the scholar to explore mass spectral:mass spectrographic shower nozzle was integrated on the chip, the mode that each is own separately, but all need extra operation relative complex, be difficult for grasping.
Aspect commercialization, micro-fluidic chip has various business-like chip listings successively, comprise lectin chip, antibody chip etc., aspect the chip mass spectrometry, Agilent company has released its chip mass spectrometer system at first, be that electron spray nozzle needle device is integrated in above the chip itself, although Sensitivity Stability is all fine, price is also relatively more expensive.In order to address such a problem, the chip path is revised in a kind of easy need not of the present invention, can finish sample ionization in the passage, and be used for the technique device of mass spectrophotometry, simple to operate, with low cost, do not need extra processing chip system just can well finish Mass Spectrometer Method.
Summary of the invention
The shortcoming of prior art the object of the present invention is to provide a kind of devices and methods therefor for the direct electron spray ionisation of sample on the micro-fluidic chip in view of the above, is existing problem in the mass spectrometry in order to solve existing micro fluidic device.
Reach for achieving the above object other relevant purposes, the invention provides a kind of device for the direct electron spray ionisation of sample on the micro-fluidic chip, this device comprises at least:
Be used for placing the three-dimensional manipulating platform of micro-fluidic chip;
The electrode of spray voltage is provided; This electrode is fixed on micro-fluidic chip inside, or places outside the chip, the independent setting;
The pulsed high voltage generator of spray voltage is provided, in order to produce induced charge in the solution in the microchannel that in the charge and discharge process, makes micro-fluidic chip, sprays thereby form;
And be arranged at the other mass spectrum of ionization device, be used for mass spectrophotometry.
In this device, the interior liquid of described electrode and micro-fluidic chip passage does not occur directly to contact.
In this device, described pulsed high voltage generator is direct current pulse power source, and output mode can be single pulse or continuous impulse.
In this device, need not to install nozzle needle additional or revise the chip channel design at chip.
The present invention comprises that also concrete steps are for the mass spectrometric analysis method of the direct electron spray ionisation of sample on the micro-fluidic chip:
The electrode that (1) will be connected with high-voltage pulse power source places the back side (chip front side is towards the mass spectrum injection port) of micro-fluidic chip microchannel outlet, in electrode and the passage between solution apart from being 0.5 ~ 2mm;
(2) regulate the three-dimensional manipulating platform, the micro-fluidic chip outlet is adjusted to apart from mass spectrum injection port 5 ~ 10mm;
(3) fluid sample is passed in the micro-fluidic chip;
(4) high-voltage pulse signal is provided for described electrode, forms electric capacity between solution in electrode and the passage; In the charge and discharge process, the solution surface of channel exit produces a large amount of electric charges, and the electron spray phenomenon occurs, thereby the sample in the ionization microchannel carries out mass spectrophotometry.
The present invention need not to revise the via design in the chip, can finish the ionization of sample in the passage and be used for mass spectrophotometry.Simple to operate, with low cost, need not the coupling that extra processing chip just can well be realized micro-fluidic chip technology and analytical technique of mass spectrum.
Description of drawings
Fig. 1 is apparatus of the present invention structural diagrams.Wherein, (a) be the device schematic diagram of the direct electron spray ionisation of sample on the micro-fluidic chip of the present invention; (b) for electrode places outside the chip, the independent schematic diagram that arranges; Device schematic diagram when (c) being fixed on micro-fluidic chip inside for electrode.
Fig. 2 is another device schematic diagram for the direct electron spray ionisation of sample on the micro-fluidic chip of the present invention.
Fig. 3 is the present invention when not adopting the design of sample cell in the exit, microchannel, is used for the device schematic diagram of the direct electron spray ionisation of sample on the micro-fluidic chip.
Fig. 4 is the present invention when being designed to groove in the microchannel, interrupts extracting the device schematic diagram that is used for the direct electron spray ionisation of sample on the micro-fluidic chip of sample ionization from groove.
Number in the figure: 1 is high-voltage pulse power source, and 2 is electrode, and 3 is micro-fluidic chip, and 4 is the microchannel, and 5 is mass spectrum, and 6 is platform, and 7 is insulation course.
Embodiment
Below by instantiation explanation embodiments of the present invention, those skilled in the art can understand other advantages of the present invention and effect easily by the disclosed content of this instructions.The present invention can also be implemented or be used by other different embodiment, and the every details in this instructions also can be based on different viewpoints and application, carries out various modifications or change under the spirit of the present invention not deviating from.
Consult Fig. 1 to shown in Figure 4.Need to prove, the diagram that provides in the present embodiment only illustrates basic conception of the present invention in a schematic way, satisfy only show in graphic with the present invention in relevant assembly but not component count, shape and size drafting when implementing according to reality, kenel, quantity and the ratio of each assembly can be according to the random changes of needs during its actual implements, and its assembly layout kenel also may be more complicated.
In order to realize a kind of micro-fluidic chip design that can need not to change, can realize preferably the method and apparatus of microflow control technique and mass-spectrometric technique coupling, the invention provides a kind of pulse power that utilizes, need not fluid sample directly contacts in electrode and the passage mass spectrum electron-spray ionization device and mass spectrometric analysis method thereof.This device is simple to operate, with low cost, can finish preferably the coupling of various types of micro-fluidic chips and analytical technique of mass spectrum.
The present invention relates to a kind of easy need not and revise the chip path, can finish sample ionization in the passage, and be used for the technique device of mass spectrophotometry, simple to operate, with low cost, do not need extra processing chip system just can well finish Mass Spectrometer Method.Device involved in the present invention mainly comprises: the three-dimensional manipulating platform of placing micro-fluidic chip; Electrode and the pulsed high voltage generator of spray voltage are provided; The described electrode of spray voltage that provides does not occur directly to contact with liquid in the micro-fluidic chip; And the mass spectrum that is arranged on the ionization device side.
Described micro-fluidic chip can be fixed on the three-dimensional regulation platform, regulates the position between its exit, microchannel and mass spectrum, so that channel outlet is in suitable position, can make the sample of ionization enter preferably mass spectrophotometry after spraying forms.This device uses the high-voltage power supply that can produce pulse direct current, and output frequency is 1 Hz ~ 10 kHz, and output voltage is at 3 ~ 15 kV, and concrete output frequency and output voltage need to regulate according to institute's analytic sample kind and flow velocity etc. are concrete.Described micro-fluidic chip need be selected preferably material of insulativity, in the time of near solution in the passage flows to the exit, forms electric capacity between solution and the electrode.
A kind of mass spectrometric analysis method for the direct electron spray ionisation of sample on the micro-fluidic chip, concrete steps are:
The electrode that 1) will be connected with high-voltage pulse power source places the back side (chip front side is towards the mass spectrum injection port) of chip microchannel outlet, in electrode and the passage between solution apart from being 0.5 ~ 2mm;
2) regulate the three-dimensional manipulating platform, the chip outlet is adjusted to apart from mass spectrum injection port 5 ~ 10mm;
3) described fluid sample is passed in the micro-fluidic chip;
4) high-voltage pulse signal is provided for described electrode, forms electric capacity between solution in electrode and the passage.In the charge and discharge process, the solution surface of channel exit produces a large amount of electric charges, and the electron spray phenomenon occurs, thereby the sample in the ionization microchannel carries out mass spectrophotometry.
As shown in Figure 1, micro-fluidic chip 3 is fixed on its three-dimensional regulation platform 6.Regulate the three-dimensional regulation platform, make the outlet of its microchannel 4 be positioned at front the 5 ~ 10mm of the injection port place of mass spectrum 5, so that preferably ionization when ionizing.Testing liquid is passed into sample microchannel 4, liquid is transported to the exit of microchannel.Make pulse power supply 1, the high-voltage signal of output pulse direct current is to pole plate 2, and output frequency is 1 Hz ~ 10 kHz, and output voltage is at 3 ~ 15 kV, and concrete output frequency and output voltage need to regulate according to institute's analytic sample kind and flow velocity etc. are concrete.
When power supply 1 is in the rising edge of pulse output, solution can (be assembled negative charge near the electrode place because charging forms electrostatic double layer, assemble positive charge away from the electrode place), a large amount of positive charges can be assembled in the exit, microchannel near mass spectrum injection port (the injection port earthing of casing), and under the effect of surface tension and coulomb repulsion, form the Taylor centrum, electron spray occurs, thereby makes the sample molecule positively charged in the solution.When power supply 1 was in the negative edge of pulse output, the positive charge that gathers on the electrode 2 can flow through the resistance (adopting 500M Ω in this device) of ground connection, finishes discharge.In discharge process, the solution in the passage can gather negative charge at channel exit.On the battery lead plate discharge time shorter, the negative charge that assemble in the exit, microchannel will be more.At this moment, just easily make sample molecule electronegative.
As mentioned above, this device can make testing sample alternately produce positive ion and negative ion in the mode of pulse.If the mass spectrum 5 of institute's coupling places the positive ion detecting pattern, then can detect the positive ion signal of sample in the passage; If mass spectrometer places the negative ion detecting pattern, but the negative ion signal of test sample then.(or can switch fast) carries out the positive and negative ion mode detection if the mass spectrometer of institute's coupling has simultaneously, and positive and negative ion detects in then can producing sample in the lump.
The present embodiment and embodiment 1 device is similar, and difference only is that the design in exit, microchannel of micro-fluidic chip of institute's coupling is from different shown in the example 1.As shown in Figure 2, all there is opening in the little pond of the sample in exit, microchannel at the upper and lower faces of chip.Need this moment at electrode 2 surperficial coated insulation layer 7(thickness 0.5mm ~ 2mm).The electrode 2 that is coated with insulation course 7 is placed an end of microchannel outlet, the other end points to the mass spectrum injection port.As implement as described in the example 1, sample under the effect of the pulse high-voltage that power supply 2 is exported, produces sample ions after sample microchannel 4 flows into the little pond of sample, detect for mass spectrum 5.
The present embodiment and embodiment 1 device is similar, and difference only is that the design in exit, microchannel of micro-fluidic chip of institute's coupling is from different shown in the example 1.The design of not adopting the little pond of sample in the exit of sample microchannel 4, sample are directly flowed out in the microchannel.At this moment, as shown in Figure 3, electrode 2 need be placed near the chip sides 4 exits, sample microchannel.As implement as described in the example 1, sample under the effect of the pulse high-voltage that power supply 2 is exported, produces sample ions after sample microchannel 4 flow to channel exit, detect for mass spectrum 5.
The present embodiment and embodiment 1 device is similar, and difference only is that the design of microchannel of micro-fluidic chip of institute's coupling is from different shown in the example 1.As shown in Figure 3, sample microchannel 4 is the open type groove on this kind chip.The present invention also can the stage casing of this kind passage to passage in liquid carry out desorb and ionization.At this moment, electrode 2 need the corresponding chip back position of the section of being placed on and sampling.As described in embodiment one, when sample is flowed through the sampling section through sample microchannel 4, under the pulse high-voltage effect of power supply 2 outputs, produce sample ions, detect for mass spectrum 5.
As described in above-mentioned embodiment 1～example 4, the present invention can utilize the charge and discharge process to electrode of high voltage pulse near the micro-fluidic chip exit, make solution example need not directly to contact with electrode and can make sample generation electron spray, thereby ionized sample is carried out Mass Spectrometer Method.In the method, charged electrode does not directly contact with solution to be measured, can be because the original function that chemical reaction affects micro-fluidic chip does not occur on the electrode.In addition, this device can adapt to the via design of the micro-fluidic chip of various ways, need not the sample channel of micro-fluidic chip is carried out extra modification, can realize preferably the coupling of micro-fluidic chip technology and analytical technique of mass spectrum
In sum, the present invention has effectively overcome various shortcoming of the prior art and the tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not is used for restriction the present invention.Any person skilled in the art scholar all can be under spirit of the present invention and category, and above-described embodiment is modified or changed.Therefore, have in the technical field under such as and know that usually the knowledgeable modifies or changes not breaking away from all equivalences of finishing under disclosed spirit and the technological thought, must be contained by claim of the present invention.
Claims (6)
1. a device that is used for the direct electron spray ionisation of sample on the micro-fluidic chip is characterized in that, this device comprises at least:
Be used for placing the three-dimensional manipulating platform of micro-fluidic chip;
The electrode of spray voltage is provided; This electrode is fixed on micro-fluidic chip inside, perhaps places outside the chip, the independent setting;
The pulsed high voltage generator of spray voltage is provided, in order to produce induced charge in the solution in the microchannel that in the charge and discharge process, makes micro-fluidic chip, sprays thereby form;
And be arranged at the other mass spectrum of ionization device, be used for mass spectrophotometry.
2. the device for the direct electron spray ionisation of sample on the micro-fluidic chip according to claim 1, it is characterized in that: described electrode for spray voltage is provided does not occur directly to contact with the liquid of micro-fluidic chip.
3. the device for the direct electron spray ionisation of sample on the micro-fluidic chip according to claim 1, it is characterized in that: described power supply is the DC pulse high-voltage power supply, output mode is single pulse or continuous impulse.
4. the device for the direct electron spray ionisation of sample on the micro-fluidic chip according to claim 1, it is characterized in that: the output frequency of described DC pulse high-voltage power supply is 1 Hz ~ 10 kHz, and output voltage is 3 ~ 15 kV.
5. the device for the direct electron spray ionisation of sample on the micro-fluidic chip according to claim 1, it is characterized in that: described power supply is AC power.
6. one kind is adopted the described device of one of claim 1-4 for the mass spectrometric analysis method of the direct electron spray ionisation of sample on the micro-fluidic chip, it is characterized in that concrete steps are:
The electrode that (1) will be connected with high-voltage pulse power source places the back side of micro-fluidic chip microchannel outlet, and micro-fluidic chip is just facing to the mass spectrum injection port, in electrode and the passage between solution apart from being 0.5 ~ 2mm;
(2) regulate the three-dimensional manipulating platform, the micro-fluidic chip outlet is adjusted to apart from mass spectrum injection port 5 ~ 10mm;
(3) fluid sample is passed in the micro-fluidic chip;
(4) high-voltage pulse signal is provided for described electrode, forms electric capacity between solution in electrode and the passage; In the charge and discharge process, the solution surface of channel exit produces a large amount of electric charges, and the electron spray phenomenon occurs, thereby the sample in the ionization microchannel carries out mass spectrophotometry.
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Cited By (6)
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| CN109331893A (en) * | 2018-11-22 | 2019-02-15 | 复旦大学 | Micro-fluidic free flow paper chromatography array electrospray mass spectrometry combined apparatus |
| CN110060916A (en) * | 2019-04-09 | 2019-07-26 | 武汉大学 | A kind of mass spectrometer for the online photochemical reaction research of high-throughput drop |
| CN110491768A (en) * | 2019-09-17 | 2019-11-22 | 中国科学院成都生物研究所 | A kind of microballon electron spray array high throughput analysis device and method |
| CN111308000A (en) * | 2020-03-24 | 2020-06-19 | 宁波大学 | Mass spectrometry system based on electrospray |
| CN114496717A (en) * | 2022-01-18 | 2022-05-13 | 中国科学院成都生物研究所 | Electrospray excitation device and ionization method |
| WO2022247246A1 (en) * | 2021-05-28 | 2022-12-01 | 深圳先进技术研究院 | Sample loading device for mass spectrometer |
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