CN107238654B - Ionization device - Google Patents
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- CN107238654B CN107238654B CN201710383180.XA CN201710383180A CN107238654B CN 107238654 B CN107238654 B CN 107238654B CN 201710383180 A CN201710383180 A CN 201710383180A CN 107238654 B CN107238654 B CN 107238654B
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- G01N27/68—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 electric discharge to ionise a gas
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Abstract
The invention discloses an ionization device. It includes: a sample capillary, an auxiliary liquid capillary and an atomizing gas capillary; a sample capillary tube, an auxiliary liquid capillary tube and an atomizing air capillary tube are arranged from inside to outside on the same axis, one end of the sample capillary tube is a direct sample introduction interface, and the other end of the sample capillary tube is a sample outlet; the sample capillary near direct sample injection interface section and the auxiliary liquid capillary pass through the T-shaped tee 1, and the sample capillary far direct sample injection interface section, the auxiliary liquid capillary and the atomized gas capillary pass through the T-shaped tee 2; an auxiliary liquid interface arranged on the auxiliary liquid capillary tube is connected with an auxiliary liquid injection tube through a vertical port of the T-shaped tee 1; an atomization gas interface arranged on the atomization gas capillary is connected with an atomization gas injection pipe through a vertical port of a T-shaped tee joint 2; an ionization high-voltage interface is arranged on the sample capillary, and an electrode of a high-voltage power supply is connected with the ionization high-voltage interface. The invention has simple structure; the ionization efficiency is high, the salt effect is avoided, and the signal-to-noise ratio of a high mass spectrum signal is obtained.
Description
Technical Field
The invention relates to an ionization device, and belongs to the field of organic spectrum analysis.
Background
Mass spectrometry is a means of ionizing a substance and characterizing the substance by determining the ion mass-to-charge ratio. Since the macroscopic material is mostly neutral or nearly neutral, the material cannot be separated by the action of an electric field or a magnetic field to generate an ion current to be detected. Therefore, the sample needs to be ionized before entering the mass spectrometry for detection, and then enters the mass spectrometry for detection. An electrospray ionizer (ESI) is a conventional ion source. The device is mainly applied to a liquid chromatogram-mass spectrometer, not only serves as an interface device between the liquid chromatogram and a mass spectrometer, but also serves as an ionization device. The electrospray nozzle mainly comprises an electrospray nozzle consisting of a plurality of layers of sleeves, wherein the innermost layer is liquid chromatogram effluent, the outer layer is jet gas, the jet gas usually adopts large-flow nitrogen, and the function of the jet gas is to enable the jetted liquid to be easily dispersed into micro-droplets. The surface charge density gradually increases during the evaporation of the droplets, and when the surface charge density increases to a certain critical value, coulomb explosion is generated, and ions can be evaporated from the surface. Subsequently, the sample is passed through the sampling hole into the analyser for ionisation by means of a voltage between the nozzle and the cone. In this process, the evaporation of the solvent is a critical step that limits the ionization efficiency, and the evaporation rate of the solvent is also one of the conditions that limit the ionization efficiency. Meanwhile, the existence of a solution salt system can inhibit the ionization process or generate high background, reduce the signal-to-noise ratio of mass spectrum signals and even lead to the blockage of capillary tubes by crystallized salt to interrupt the signals.
Disclosure of Invention
The invention aims to provide an ionization device, which has the advantages of simple structure, simple assembly and maintenance and high-integration manufacturing; when the ionic liquid is applied, a polar solvent can be mixed into a system while spraying, so that the ionization efficiency is effectively improved, and the influence of a salt effect in a sample on ionization is avoided; and obtaining the signal-to-noise ratio of the higher mass spectrum signal.
The invention provides an ionization device, comprising: the device comprises a sample capillary tube, an auxiliary liquid capillary tube, an atomized gas capillary tube and a high-voltage power supply;
arranging the sample capillary tube, the auxiliary liquid capillary tube and the atomizing gas capillary tube from inside to outside by adopting the same axis;
one end of the sample capillary is a direct sample inlet, and the other end of the sample capillary is a sample outlet;
the sample capillary close to the direct injection interface section and the auxiliary liquid capillary pass through a T-shaped tee 1, and the sample capillary far from the direct injection interface section, the auxiliary liquid capillary and the atomizing air capillary pass through a T-shaped tee 2;
an auxiliary liquid interface is arranged on the auxiliary liquid capillary tube, wherein one end of the auxiliary liquid capillary tube is an auxiliary liquid outlet, and the auxiliary liquid interface is connected with an auxiliary liquid injection tube through a vertical port of the T-shaped tee 1;
an atomization gas interface is arranged on the atomization gas capillary tube, wherein one end of the atomization gas capillary tube is an atomization gas outlet, and the atomization gas interface is connected with an atomization gas injection pipe through a vertical port of the T-shaped tee joint 2;
an ionization high-voltage interface is arranged on the sample capillary, and an electrode of the high-voltage power supply is connected with the ionization high-voltage interface.
In the invention, the direct sample introduction interface of the sample capillary is connected with the sample cell;
the tee is not a mixing device, and is a structure which allows liquid and gas to be in concentric space.
In the present invention, depending on the characteristics of the sample, a high voltage power supply (including electrodes) may be directly inserted into the sample cell or the electrodes of the high voltage power supply built in the sample capillary as described above may be provided to apply the spray voltage. And (3) ventilating and repeatedly adjusting the position of the sample capillary in the spray head to enable the sample capillary to generate Venturi self-suction effect to spray out the sample in a stable droplet shape, and completing debugging.
The ionization device further comprises an ionization high-pressure interface, and the ionization high-pressure interface is connected with the atomization gas interface; the ionization high-voltage interface is in contact with the solution in the ionization device, and the electrode can be directly connected with the reaction system due to the fact that the water phase system has high conductivity.
When the ionization device is used for mass spectrometry, the ionization device also comprises a high-voltage power supply, and the high-voltage power supply is connected with the ionization voltage interface.
In the ionization device, the atomization gas outlet of the atomization gas capillary is closed, and the position of the atomization gas outlet of the atomization gas capillary can be adjusted according to different samples;
the sample capillary and the auxiliary liquid capillary are both made of quartz, the sample capillary can be a quartz capillary with an outer diameter of 365 μm and an inner diameter of 250 μm, and the auxiliary liquid capillary can be a quartz capillary with an inner diameter of 530 μm and an outer diameter of 690 μm;
the atomizing gas capillary is made of glass, and the inner diameter of the atomizing gas capillary can be 1 mm.
In the invention, the sample capillary, the auxiliary liquid capillary and the atomizing air capillary are arranged into a three-layer sleeve structure, a sample is mixed with auxiliary liquid during ionization, and salts cannot be separated out in a pipeline; has the function of sample self-suction.
The ionization device further comprises a quantitative mechanical pump, wherein the quantitative mechanical pump is connected with the auxiliary liquid interface through a pipeline; the quantitative mechanical pump is used for introducing auxiliary liquid and can be used for sample flow rate modulation; the material of the pipeline can be selected from materials known in the art, preferably a material with good strength and toughness, and chemical inertness meets the test requirement, and can be polytetrafluoroethylene specifically.
When the ionization device is used for an open reaction system, the ionization device also comprises a throttle valve and a flowmeter accessory;
the throttling valve is arranged on a pipeline of the atomizing air interface;
the flow meter accessory is connected with the atomizing air interface through a pipeline; the material of the pipeline can specifically adopt polyvinyl chloride;
when the ionization device is used for a closed reaction system, the ionization device also comprises an injection sample introduction adapter;
the injection sample introduction adapter is of a two-way structure, one end of the two-way structure is connected with the outer diameter of the sample capillary in a matching mode, and the other end of the two-way structure is connected with an output port of an injection pump or a peristaltic pump.
When the ionization device is used for an open type reaction system, the ionization device also comprises a pressure reducing valve, and the pressure reducing valve is arranged on a pipeline of the atomization gas interface.
The ionization device is applied to the ionization device for detecting a sample, and the sample detection method is characterized by specifically adopting a spectrum.
The spectra in the above application may specifically be mass spectra.
The ionization device is applied to the spectrum characterization and/or solution detection of a sample which can generate chemical reaction with the auxiliary liquid.
In the present invention, the spectrum may be a mass spectrum.
The invention further provides a method for detecting mass spectra, which comprises the following steps:
1) assembling each part according to the requirement to obtain the ionization device;
2) increasing the flow speed of the atomization airflow to a design value;
3) adjusting the sample capillary to the maximum fog amount by using an automatic lifting sample introduction mode;
4) maximize the auxiliary liquid flow, slowly increase the voltage to the total ion count of 1 × 103The above;
5) optimizing mass spectrometer scanning parameters;
6) optimizing the flow rate of the auxiliary liquid;
7) mass spectrometric detection of the sample was started.
The invention has the following advantages:
by utilizing the ionization device, the system can be mixed with the organic solvent while spraying, and the mass spectrum ion signal of the aqueous phase solution is effectively improved. And because the mixing position is outside the spray outlet, the sample which is not sprayed is not changed at all. In a high salinity sample, the salting-out phenomenon caused by the polarity change of the solvent can be completely avoided, the nozzle is prevented from being blocked, and the ionization efficiency is improved. The ionization device is simple in structure, simple in assembly and maintenance and capable of being manufactured in a highly integrated mode. When the aqueous solution signal is lifted, the sample can be automatically lifted by utilizing the air flow, and the sample can be injected by using a pump. The flow rate is fast when the sample is automatically lifted, the analysis delay is low, and the method can be used for on-line monitoring of the reaction. The signal-to-noise ratio of a high mass spectrum signal can be obtained, and reaction intermediates which cannot be found before can be easily found. When the auxiliary liquid is closed, the structure function of the auxiliary liquid is consistent with that of the commercial electric spray ion source, and the application range of the original ion source is expanded.
Drawings
Fig. 1 is a schematic structural diagram (a) and a schematic device diagram (b) of a co-spray ion source.
The individual components in fig. 1(a) are labeled as follows:
1, a high-voltage electrode; 2, a sample pool; 3 a sample capillary; 4 auxiliary liquid injection pipe; 5, a tee joint 1; 6 auxiliary liquid capillary; 7 an atomized gas injection pipe; 8, a tee joint 2; 9 atomizing the air capillary.
FIG. 2 is a schematic diagram showing the detailed structure of the ion shower head in FIG. 1 (numerical unit: mm).
FIG. 3 is the aqueous signal for different substances, where FIG. 3(a) is citric acid (negative mode), FIG. 3(b) is p-nitrobenzoic acid (negative mode), where FIG. 3(c) is sodium dodecylsulfate (negative mode), FIG. 3(d) is glycine (negative mode), where FIG. 3(e) is glycine (positive mode), and FIG. 3(f) is the ESI signal for different substances (not enhanced) compared to the signal intensity of the device described in this patent (enhanced).
Fig. 4 is an on-line analysis signal, in which fig. 4(a) is gluconic acid without using a methanol optimization signal, and fig. 4(b) is gluconic acid after using a methanol optimization signal.
FIG. 5 is a diagram showing an example of the spectral purification, wherein FIG. 5(a) is a mass spectrum of the reaction system and FIG. 5(b) is a graph showing the time-dependent tendency of the signals of the reactants, intermediates and products in the reaction.
FIG. 6 is an example of ionization of an unstable reaction intermediate, in which FIG. 6(a) is a mass spectrum of a mixed solution of glucose and FAD detected using the apparatus described in the patent, and FIG. 6(b) is a mass spectrum of a mixed solution of glucose and FAD detected using a commercial ESI ion source.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Methanol (HPLC grade) was purchased from spectrochemistry ltd (barrenrelix, germany). The other reagents were Sigma-Aldrich (USA) and required to be BR or AR.
The water used in the experiment process is ultrapure water, and is processed by a Milli-Q ultrapure water purification system. The high-purity nitrogen gas is purchased from the gas sales center of the Beijing millennium Jingcheng.
The apparatus used in the following examples: LTQ linear ion trap mass spectrometer (Thermo Fisher Scientific, usa); 0.9-1.1 × 100mm glass spotting capillary was purchased from Shanghai great wall scientific instruments, and quartz capillary was purchased from Jiangxi chromatograph devices, Inc. of Yongnian.
The capillary tube closing is a manual operation, the tail end of the sample application capillary tube is burned and closed by flame, and then the sample application capillary tube is ground by No. 100 abrasive paper to a proper opening size and polished by No. 500 abrasive paper. The remaining lines are assembled as shown in figure 1. After the assembly was completed, 1.5L/min of nitrogen gas was introduced, the position of the end of the innermost capillary was adjusted, and the other end was placed in a solution of methanol-water 1:1(v/v) until the liquid could be ejected naturally and stably.
In the whole experiment process, except that the spraying voltage is manually adjusted, the temperature of the vacuum interface is constant at 200 ℃, and other test parameters are automatically optimized and determined by software.
Example 1 ionization apparatus
As shown in fig. 1-2, the ionization apparatus of the present invention comprises: a sample capillary 3, an auxiliary liquid capillary 6 and an atomizing air capillary 9; the sample capillary 3, the auxiliary liquid capillary 6 and the atomizing gas capillary 9 are arranged from inside to outside on the same axis. One end of the sample capillary 3 is a direct sample inlet interface (connected with the sample cell 2), and the other end is a sample outlet; the sample capillary 3 near the direct sample inlet section and the auxiliary liquid capillary 6 pass through the T-shaped tee 15, the sample capillary 3 far from the direct sample inlet section, the auxiliary liquid capillary 6 and the atomized gas capillary 9 pass through the T-shaped tee 28, and the three layers of sleeves are arranged, so that the sample can be mixed with the auxiliary liquid during ionization, and salts can not be separated out in a pipeline, and the sample has a self-absorption function; an auxiliary liquid interface is arranged on the auxiliary liquid capillary tube 6, wherein one end of the auxiliary liquid capillary tube 6 is an auxiliary liquid outlet, and the auxiliary liquid interface is connected with the auxiliary liquid injection tube 4 through a vertical port of a T-shaped tee 15; an atomizing air interface is arranged on the atomizing air capillary 9, wherein one end of the atomizing air capillary 9 is an atomizing air outlet, and the atomizing air interface is connected with the vertical port of the T-shaped tee 28 and the atomizing air injection pipe 7. An ionization high-voltage interface is arranged on the sample capillary 3, and a high-voltage electrode 1 of a high-voltage power supply is connected with the ionization high-voltage interface.
Furthermore, an atomizing gas outlet of an atomizing gas capillary 9 in the ionization device is in a closing-in arrangement, and the position of the atomizing gas outlet of the atomizing gas capillary 9 can be adjusted according to different samples;
the sample capillary and the auxiliary liquid capillary are both made of quartz, the sample capillary can be a quartz capillary with an outer diameter of 365 mu m and an inner diameter of 250 mu m, and the auxiliary liquid capillary can be a quartz capillary with an inner diameter of 530 mu m and an outer diameter of 690 mu m;
the atomizing air capillary 9 is made of glass, and the inner diameter of the atomizing air capillary can be 1 mm.
Furthermore, the ionization device also comprises a quantitative mechanical pump which is connected with the auxiliary liquid interface through a polytetrafluoroethylene pipeline; the quantitative mechanical pump is used for introducing auxiliary liquid and can be used for sample flow rate modulation.
When the ionization device is used for an open reaction system, the ionization device also comprises a throttle valve and a flowmeter accessory; the throttle valve is arranged on a pipeline of the atomizing air interface; the flow meter accessory is connected with the atomizing gas interface through a polyvinyl chloride pipeline;
when the ionization device is used for a closed reaction system, the ionization device also comprises an injection sample introduction adapter; the injection sample introduction adapter is of a two-way structure, one end of the two-way structure is connected with the outer diameter of the sample capillary in a matching mode, and the other end of the two-way structure is connected with an output port of an injection pump or a peristaltic pump.
When the ionization device is used for an open reaction system, the ionization device also comprises a pressure reducing valve, and the pressure reducing valve is arranged on a pipeline of an atomization gas interface.
Example 2 Signal amplification of citric acid solution
The ionization device in embodiment 1 of the present invention is applied to a citric acid solution, and specifically, the following is applied:
solution preparation: a 10ppm citric acid solution was prepared using 100mM pH 7.2 ± 0.2 mixed phosphate buffer solution as a base.
The test mode is a negative ion mode. The sample was injected using a syringe pump at a flow rate of 3.5. mu.L/min. The spray voltage was 0.40 kV. The methanol flow rate was 80. mu.L/min. The signal of fig. 3(a) is obtained. It can be seen that the molecular ion peak increases approximately 1-fold in intensity when methanol is turned on. It is demonstrated that the ionizer of the present invention is suitable for the ionization of acidic solutions.
Example 3 Signal amplification of p-Nitrobenzoic acid alkaline solution
The ionization device in embodiment 1 of the present invention is applied to p-nitrobenzoic acid alkaline solution, and specifically comprises the following steps:
solution preparation: sodium hydroxide was added to promote dissolution of benzoic acid, and a 100ppm solution (in terms of benzoic acid) was directly prepared using ultrapure water.
The test mode is a negative ion mode. The sample was injected using a syringe pump at a flow rate of 1.0. mu.L/min. The spraying voltage was 0.30kV, and the flow rate of methanol was 80. mu.L/min, whereby the signal of FIG. 3(b) was obtained. It can be seen that the molecular ion peak intensity of the sample is raised to about 10 times when methanol is turned on. The ionizer was shown to be suitable for the ionization of alkaline solutions.
Example 4 Signal amplification of Sodium Dodecyl Sulfate (SDS) and salt-containing solution
The ionization device in embodiment 1 of the present invention is applied to Sodium Dodecyl Sulfate (SDS) and salt-containing solution, and specifically includes the following:
solution preparation: a 10ppm sodium lauryl sulfate solution was prepared using 100mM pH 7.2 ± 0.2 mixed phosphate buffer solution as a base.
The test mode is a negative ion mode. The sample was injected using a syringe pump at a flow rate of 1.0. mu.L/min. The spraying voltage was 0.41kV and the flow rate of methanol was 40. mu.L/min, and the signal of FIG. 3(c) was obtained. It can be seen that the molecular ion peak intensity of the sample is raised to about 18 times when methanol is turned on. The condition of spray reduction or spray head blockage is not found in the whole process, and no crystallization is generated at the spray head, which indicates that the ionization device of the invention is completely salt-resistant.
Example 5 Signal amplification of Glycine ampholyte
The ionization device in the embodiment 1 of the invention is applied to glycine ampholyte, and the following concrete steps are carried out:
solution preparation: a 10ppm glycine solution was prepared using 100mM pH 7.2 ± 0.2 mixed phosphate buffer solution as a base.
The sample was injected using a syringe pump at a flow rate of 1.0. mu.L/min. The spray voltage was 0.71kV, the methanol flow rate was 40. mu.L/min, and the signals of FIG. 3(d) and FIG. 3(e) were obtained using the negative ion mode and the positive ion mode, respectively. It can be seen that the cationic and anionic peak intensities of the sample molecules are respectively raised to about 18 times and about 24 times when methanol is turned on. The ionization device of the invention can be used for detecting ampholytes.
Example 6 non-ionic Peak removal of gluconic acid
The ionization device in the embodiment 1 of the invention is applied to the removal of non-molecular ion peaks of gluconic acid, and specifically comprises the following steps:
solution preparation: a 1mM gluconic acid solution was prepared using a 100mM pH 7.2 ± 0.2 mixed phosphate buffer solution as a base.
The test mode is a negative ion mode. The sample was injected using a syringe pump at a flow rate of 5. mu.L/min. The spraying voltage was 1.12kV, and the flow rate of methanol was 40. mu.L/min, whereby the signal of FIG. 4(b) was obtained. It can be seen that the intensity of the non-ionic peak was reduced to about 4% of that which was not removed when methanol was turned on, relative to the case where methanol was not turned on (fig. 4 (a)). It is demonstrated that the ionization apparatus of the present invention can reduce the interference.
Example 7 on-line reaction monitoring of the enzymatic Oxidation of Glucoase
The ionization device in the embodiment 1 of the invention is applied to the glucose enzyme catalytic oxidation, and the specific steps are as follows:
solution preparation: the reaction solution contained 200mM glucose, 10mM pH 7.2 phosphate buffer system, and 230U glucose oxidase.
Samples were injected using the auto-extraction function of the ionizer. The flow rate of methanol is 50 mu L/min, the ionization voltage is 2.2kV, the reaction system is heated by using a constant-temperature water bath, air is blown into the reaction system by using a compression pump, and the spectrogram is recorded while enzyme is added. The signal shown in fig. 5 is obtained. The molecular ion peak intensity of the gluconic acid is increased along with the increase of the reaction time, which indicates that the ionization device can be used for on-line monitoring of the reaction.
Example 8 intermediate assay for glucose Oxidation
The ionization device in the embodiment 1 of the invention is applied to the intermediate detection of glucose oxidation, and the specific steps are as follows:
solution preparation: each 10mL of the reaction solution contained 10ppm glucose and 7ppm FAD, 230U glucose oxidase.
Samples were injected using a syringe at a rate of 50 μ L/min. The flow rate of methanol was 50. mu.L/min, and the ionization voltage was 2.2kV, whereby the signal shown in FIG. 6(a) was obtained. Comparison with the spectrum 6(b) obtained by commercial ESI shows that the intermediate excimer ion peak appears, whereas the ion peak of the intermediate is not obtained by ordinary ESI. The ionization device of the invention has milder ionization effect.
Claims (9)
1. An ionization apparatus, comprising: the device comprises a sample capillary tube, an auxiliary liquid capillary tube, an atomized gas capillary tube and a high-voltage power supply;
the sample capillary, the auxiliary liquid capillary and the atomizing air capillary are arranged from inside to outside on the same axis,
one end of the sample capillary is a direct sample inlet, and the other end of the sample capillary is a sample outlet;
the sample capillary close to the direct injection interface section and the auxiliary liquid capillary pass through a T-shaped tee 1, and the sample capillary far from the direct injection interface section, the auxiliary liquid capillary and the atomizing air capillary pass through a T-shaped tee 2;
an auxiliary liquid interface is arranged on the auxiliary liquid capillary tube and is connected with an auxiliary liquid injection tube through a vertical port of the T-shaped tee 1;
the atomization gas capillary is provided with an atomization gas interface, and the atomization gas interface is connected with an atomization gas injection pipe through a vertical port of the T-shaped tee joint 2;
an ionization high-voltage interface is arranged on the sample capillary, and an electrode of the high-voltage power supply is connected with the ionization high-voltage interface;
the T-shaped tee 1 and the T-shaped tee 2 are not mixing devices and are in concentric space structures for liquid and gas.
2. The ionization apparatus according to claim 1, wherein: the atomized gas outlet of the atomized gas capillary is arranged in a closing-up manner;
the sample capillary tube and the auxiliary liquid capillary tube are both made of quartz;
the atomized gas capillary is made of glass.
3. The ionization apparatus according to claim 1 or 2, wherein: the ionization device also comprises a quantitative mechanical pump, and the quantitative mechanical pump is connected with the auxiliary liquid interface through a pipeline.
4. The ionization apparatus according to claim 1 or 2, wherein: when the ionization device is used for an open reaction system, the ionization device also comprises a throttle valve and a flowmeter accessory;
the throttling valve is arranged on a pipeline of the atomizing air interface;
the flow meter accessory is connected with the atomizing air interface through a pipeline;
when the ionization device is used for a closed reaction system, the ionization device also comprises an injection sample introduction adapter;
the injection sample introduction adapter is of a two-way structure, one end of the two-way structure is connected with the outer diameter of the sample capillary in a matching mode, and the other end of the two-way structure is connected with an output port of an injection pump or a peristaltic pump.
5. The ionization apparatus according to claim 1 or 2, wherein: when the ionization device is used for an open type reaction system, the ionization device also comprises a pressure reducing valve, and the pressure reducing valve is arranged on a pipeline of the atomization gas interface.
6. Use of an ionization device as claimed in any one of claims 1 to 5 for the detection of a sample.
7. Use according to claim 6, characterized in that: the sample detection method adopts spectral characterization.
8. Use of an ionization device according to any one of claims 1 to 5 for spectroscopic characterization and/or solution detection of a sample that is capable of undergoing a chemical reaction with an auxiliary liquid.
9. A method of mass spectrometry detection comprising the steps of:
1) assembling the individual components as required to obtain an ionization device according to any one of claims 1 to 5;
2) increasing the flow speed of the atomization airflow to a design value;
3) adjusting the sample capillary to the maximum fog amount by using an automatic lifting sample introduction mode;
4) maximize the auxiliary liquid flow, slowly increase the voltage to the total ion count of 1 × 103The above;
5) optimizing mass spectrometer scanning parameters;
6) optimizing the flow rate of the auxiliary liquid;
7) mass spectrometric detection of the sample was started.
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| IT201700115527A1 (en) * | 2017-10-13 | 2019-04-13 | Univ Degli Studi Di Urbino Carlo Bo | MACHINE FOR CHEMICAL ANALYSIS INCLUDING THE COMBINATION OF MASS SPECTROMETRY WITH ELECTRONIC IONIZATION WITH LIQUID CHROMATOGRAPHY |
| US10658168B2 (en) | 2018-05-03 | 2020-05-19 | Perkinelmer Health Sciences Canada, Inc. | Multiple gas flow ionizer |
| CN109357991B (en) * | 2018-09-27 | 2020-05-26 | 清华大学 | Mass spectrum flow cytometry sample introduction and ionization device based on marking-free principle |
| CN110459459A (en) * | 2019-07-29 | 2019-11-15 | 中国科学院上海有机化学研究所 | A kind of ion induction electrospray ionisation method and apparatus |
| EP4082669A4 (en) * | 2020-02-03 | 2023-10-18 | National Institute Of Advanced Industrial Science and Technology | Spray ionization device |
| CN113237981B (en) * | 2021-03-31 | 2022-04-26 | 中国科学院化学研究所 | Novel interface for living body microdialysis mass spectrometry combined real-time online analysis technology |
| CN113176325B (en) * | 2021-04-14 | 2023-05-12 | 北京师范大学 | Normal pressure mass spectrum online monitoring system for accelerating degradation of organic pollutants by plasmas in milliseconds |
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| CA2717482C (en) * | 2008-03-07 | 2016-11-22 | The University Of British Columbia | Self-contained capillary electrophoresis system for interfacing with mass spectrometry |
| CN103389336A (en) * | 2013-07-17 | 2013-11-13 | 东华理工大学 | Mass spectrometry imaging method capable of rapidly identifying of handwriting authenticity |
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