WO2023003335A1 - 액체 크로마토그래피, 이온화 장치 그리고 질량 분석기의 인터페이스 및 이를 이용한 시료 분석 방법 - Google Patents
액체 크로마토그래피, 이온화 장치 그리고 질량 분석기의 인터페이스 및 이를 이용한 시료 분석 방법 Download PDFInfo
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- WO2023003335A1 WO2023003335A1 PCT/KR2022/010577 KR2022010577W WO2023003335A1 WO 2023003335 A1 WO2023003335 A1 WO 2023003335A1 KR 2022010577 W KR2022010577 W KR 2022010577W WO 2023003335 A1 WO2023003335 A1 WO 2023003335A1
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- sample
- target
- droplet
- liquid chromatography
- mass spectrometer
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- 238000004811 liquid chromatography Methods 0.000 title claims abstract description 70
- 238000012284 sample analysis method Methods 0.000 title claims description 17
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000007921 spray Substances 0.000 claims abstract description 6
- 238000000375 direct analysis in real time Methods 0.000 claims description 19
- 230000007423 decrease Effects 0.000 claims description 9
- 239000001307 helium Substances 0.000 claims description 9
- 229910052734 helium Inorganic materials 0.000 claims description 9
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 8
- 230000001678 irradiating effect Effects 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 3
- 238000012063 dual-affinity re-targeting Methods 0.000 claims 2
- 239000000523 sample Substances 0.000 description 65
- 239000000463 material Substances 0.000 description 30
- 238000001819 mass spectrum Methods 0.000 description 17
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 14
- 239000007789 gas Substances 0.000 description 13
- 239000002210 silicon-based material Substances 0.000 description 8
- 238000000752 ionisation method Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 238000000065 atmospheric pressure chemical ionisation Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000132 electrospray ionisation Methods 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000000935 solvent evaporation Methods 0.000 description 2
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Images
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
- G01N30/724—Nebulising, aerosol formation or ionisation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
- G01N30/7273—Desolvation chambers
Definitions
- the present invention relates to an interface of a liquid chromatography, an ionizer, and a mass spectrometer, and a sample analysis method using the same, and relates to an interface of a liquid chromatography, an ionizer, and a mass spectrometer capable of effectively detecting non-polar low-molecular-weight substances and silicon-based compounds, and an interface of a liquid chromatography, an ionizer, and a mass spectrometer, and the same. It relates to the sample analysis method used.
- liquid chromatography/mass spectrometer For quantitative and qualitative analysis of substances, liquid chromatography/mass spectrometer (LC/MS) is mainly used.
- a liquid chromatography mass spectrometer (LC/MS) connects the outlet of the liquid chromatography to the inlet of the mass spectrometer to supply the mass spectrometer with a sample containing a target that has been separated into single components in the liquid chromatography, and the components of the target in the mass spectrometer. can be detected.
- a mass spectrometer separates ions generated by ionizing a target to be analyzed according to a ratio between mass and charge amount, and displays them in the form of a mass spectrum. Therefore, in a liquid chromatography mass spectrometer (LC/MS), an ionizer for ionizing a target is disposed between the liquid chromatography and the mass spectrometer.
- LC/MS liquid chromatography mass spectrometer
- Ionization methods widely used in liquid chromatography mass spectrometry include electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI).
- ESI electrospray ionization
- APCI atmospheric pressure chemical ionization
- This ionization method is widely used in liquid chromatography mass spectrometry (LC/MS) because it can effectively perform not only the role of ionizing the target (analyte) but also the interface between liquid chromatography and mass spectrometry.
- the target is a non-polar low-molecular-weight material or a silicon-based compound, it is sometimes difficult to analyze by this ionization method.
- Direct Analysis in Real Time is one of the methods capable of effectively ionizing these materials (eg, non-polar low molecular weight materials or silicon-based compounds).
- DART real-time direct analysis
- LC/MS liquid chromatography mass spectrometry
- a solvent contained in a sample eluted from liquid chromatography must be rapidly volatilized to make a target into a gas phase. Accordingly, it is necessary to develop an efficient interface for connecting DART to LC/MS.
- Embodiments of the present invention are intended to provide interfaces of liquid chromatography, ionization devices, and mass spectrometers suitable for applying real-time direct analysis to liquid chromatography mass spectrometry.
- Another embodiment of the present invention is to provide a sample analysis method using an interface according to an embodiment of the present invention.
- liquid chromatography (LC), ionizer, and mass spectrometer (MS) interfaces are provided.
- a sample containing the target eluted from the liquid chromatography is ionized by an ionizer and introduced into a mass spectrometer.
- the interface may include a droplet atomizer for converting and spraying a sample including a target eluted in liquid chromatography into a sample droplet form; an inlet tube through which the target is introduced into a mass spectrometer; and an evaporator disposed between the droplet sprayer and the inlet tube to evaporate the solvent included in the sample droplet to generate a gaseous target.
- the ionizer irradiates a beam on a gaseous target in an inlet tube to ionize the gaseous target introduced into a mass spectrometer through the inlet tube
- the evaporator includes a block capable of being heated and formed with at least one opening, A sample droplet sprayed from the sprayer passes through the at least one opening and is generated as a gaseous target, and the generated gaseous target may flow into the inlet pipe.
- One end of the at least one opening facing the droplet atomizer may be formed as an inclined surface whose diameter decreases along the flow of the sample droplet.
- a diameter or length of the at least one opening may be adjustable.
- the block may include a plurality of pieces, and the plurality of pieces may be combined with each other to form one block.
- the evaporator may further include a housing, and the block may be detachably mounted in the housing so as to cross the flow of the sample droplet.
- the diameter of one end of the opening may be 1 mm to 20 mm, the diameter of the other end of the opening may be 0.1 mm to 5 mm, and the length of the opening along the flow of the sample droplet may be 0.5 mm to 100 mm.
- the block is heated to a set temperature, and the set temperature may be 50 °C to 500 °C.
- the ionizer may be a DART irradiating a helium beam.
- the droplet atomizer may be an electric atomizer or a gas atomizer.
- a sample analysis method includes separating and eluting a sample including a target of a single component by performing liquid chromatography by liquid chromatography; converting and spraying a sample containing a target eluted from liquid chromatography by a droplet atomizer into a sample droplet form; evaporating the solvent in the sample droplets ejected from the droplet sprayer by means of an evaporator to generate a gaseous target; ionizing the gaseous target by irradiating a beam onto the gaseous target by means of an ionizer; and performing mass analysis of the ionized target by means of a mass spectrometer.
- the evaporator may include a housing and a block detachably mounted in the housing so as to intersect with the flow of sample droplets and heated to a set temperature.
- the block may include at least one opening, and a sample droplet sprayed by the droplet atomizer may pass through the at least one opening and be generated as a gaseous target, and the generated gaseous target may be introduced into a mass spectrometer through an inlet pipe.
- One end of the at least one opening facing the droplet atomizer may be formed as an inclined surface whose diameter decreases along the flow of sample droplets.
- the ionizer may be a DART that irradiates a helium beam at a gaseous target flowing within an inlet tube.
- the sample analysis method may further include adjusting a diameter or length of the opening or a set temperature according to a target.
- the diameter of one end of the aperture is 1 mm to 20 mm, the diameter of the other end of the aperture is 0.1 mm to 5 mm, the length of the aperture along the flow of the sample droplet is 0.5 mm to 100 mm, and the set temperature is 50 ° C to 500 ° C.
- the real-time direct analysis method to a liquid chromatography mass spectrometer, it is possible to effectively detect nonpolar low molecular weight substances and silicon-based compounds that are difficult to detect by conventional LC/MS using other ionization methods.
- various samples can be effectively analyzed by adjusting the diameter and length of the opening formed in the block according to the composition and injection conditions of the sample droplet including the target to be analyzed.
- FIG. 1 is a schematic diagram of a liquid chromatography mass spectrometer according to an embodiment of the present invention.
- FIG. 2 is a schematic cross-sectional view showing a block according to one example.
- FIG. 3 is a schematic cross-sectional view showing a block according to another example.
- FIG. 4 is a flowchart of a sample analysis method according to another embodiment of the present invention.
- Example 5 is a diagram showing the molecular structure of a material according to Example 1.
- Example 6 is a mass spectrum of a material according to Example 1 by a liquid chromatography mass spectrometer according to an embodiment of the present invention.
- Example 7 is a diagram showing the molecular structure of a material according to Example 2.
- Example 8 is a diagram showing the molecular structure of a material according to Example 3.
- Example 9 is a mass spectrum of a material according to Example 2 by a liquid chromatography mass spectrometer according to an embodiment of the present invention.
- Example 10 is a mass spectrum of a material according to Example 2 by a liquid chromatography mass spectrometer according to the prior art.
- Example 11 is a mass spectrum of a material according to Example 3 by a liquid chromatography mass spectrometer according to an embodiment of the present invention.
- Example 12 is a mass spectrum of a material according to Example 3 by a liquid chromatography mass spectrometer according to the prior art.
- target or a term similar thereto refers to an object to be analyzed using a liquid chromatography mass spectrometer.
- sample or similar terms are eluted in liquid chromatography, and include a solvent and a target.
- An interface of liquid chromatography (LC), ionizer, and mass spectrometer (MS) is disposed between the liquid chromatography and the mass spectrometer, and quickly detects a target included in a sample eluted from the liquid chromatography. It evaporates into a gas phase and helps ionize the gas phase target by the beam irradiated from the ionizer. Therefore, according to an embodiment of the present invention, it is possible to provide an interface suitable for applying a direct analysis method (DART) capable of effectively detecting nonpolar low molecular weight substances and silicon-based compounds to LC/MS.
- DART direct analysis method
- a sample analysis method includes the steps of rapidly evaporating a target included in a sample eluted from liquid chromatography into a gas phase by using the interface according to the embodiment of the present invention, and beaming the target to the gas phase with DART. ionizing the target by irradiating and introducing the ionized target into a mass spectrometer.
- FIG. 1 is a schematic diagram of a liquid chromatography mass spectrometer according to an embodiment of the present invention.
- the liquid chromatography mass spectrometer includes a liquid chromatography (5), a droplet atomizer (10), an evaporator (20), an inlet pipe (30), and an ionizer (40). , and a mass spectrometer 50.
- the droplet atomizer 10, the evaporator 20, and the introduction pipe 30 constitute an interface according to an embodiment of the present invention.
- Liquid chromatography (5) separates a mixture into single components by using the fact that the passage rates of the components included in the mixture are different depending on the affinity for the mobile phase and the stationary phase of the liquid phase. That is, liquid chromatography (5) separates a sample containing a target of a single component present in solution.
- the type of liquid chromatography 5 is not limited, and various types of liquid chromatography 5 known to those skilled in the art can be used.
- a droplet atomizer (10) is disposed downstream of and connected to the liquid chromatography (5).
- the droplet atomizer 10 injects a sample containing a target of a single component separated by the liquid chromatography 5 into the evaporator 20 in the form of droplets. That is, the droplet atomizer 10 injects the sample droplet X1 into the evaporator 20 .
- the droplet atomizer 10 includes a probe 12 and sprays the sample droplet X1 through the probe 12 .
- the type of droplet atomizer 10 is not limited, but may be an electric atomizer or a gas atomizer in one example.
- the solvent included in the sample can be easily evaporated in the evaporator 20.
- sheath gas may be additionally used to effectively evaporate the solvent. Usable sheath gas may be, but is not limited to, nitrogen, air, and the like.
- the evaporator 20 is disposed downstream of the droplet atomizer 10, receives the sample droplet X1 sprayed through the probe 12, and evaporates the solvent in the sample droplet X1 to a gaseous target including a target ( X2) is created.
- the evaporator 20 includes a housing 22 and a block 24.
- the housing 22 has a hollow shape, and at least a part of one surface thereof is open so that the probe 12 sprays the sample droplet X1 into the housing 22 through the open surface.
- a block 24 is disposed inside the housing 22 to cross the housing 22 and divide the housing 22 into two parts.
- the probe 12 sprays the sample droplets X1 to the first part 22a of the housing 22, and the introduction pipe 30 is connected to the second part 22b of the housing 22.
- the block 24 is detachably mounted in the housing 22 so as to cross the flow direction of the sample droplet X1, at least one opening 26 is formed, and a heating means (not shown) is installed inside or outside. ) can be heated to the set temperature.
- the sample droplets X1 sprayed onto the first part 22a of the housing 22 are deposited on the surface of the block 24 (including the opening 26) or heated and evaporated while passing through the opening 26,
- the evaporated gaseous target X2 passes through the opening 26 and moves to the second part 22b of the housing 22 .
- the gaseous target (X2) moved to the second part (22b) of the housing (22) is supplied to the mass spectrometer (50) through the inlet pipe (30).
- Block 24 will be described in more detail below with reference to FIGS. 2 and 3 .
- Figure 2 is a schematic cross-sectional view showing a block according to one example
- Figure 3 is a schematic cross-sectional view showing a block according to another example.
- the block 24 is integrally formed as one piece. At least one opening 26 is formed in the block 24 .
- One end of each opening 26 facing the probe 12 is formed with an inclined surface 28 whose diameter decreases along the flow of the sample droplet X1, and the remaining portion of the opening 26 excluding the inclined surface 28 has its diameter this can be constant. That is, the diameter of each opening 26 gradually decreases from one side to the other along the flow of the sample droplet X1 to form an inclined surface 28, and the remaining portion of each opening 26 forms an inclined surface 28. On the other side of the diameter may be constant.
- the surface area of one end of the opening 26 is increased, whereby the sample droplet X1 ejected from the probe 12 moves through the opening. (26)
- the probability of entering inside increases. As a result, more sample droplets X1 enter the opening 26 and are heated, whereby rapid and effective evaporation of the sample droplets X1 is possible.
- the diameter D1 of one end of the opening 26 may be 1 mm to 20 mm. If the diameter D1 of one end of the opening 26 is smaller than 1 mm, a sufficient amount of sample droplets X1 cannot enter the opening 26, and if the diameter D1 of one end of the opening 26 is greater than 20 mm, the opening 26 is larger than 20 mm.
- the sample droplet X1 entering (26) may not be evaporated by the block (24).
- the diameter D2 of the other end of the opening 26 may be 0.1 mm to 5 mm.
- the diameter D2 of the other end of the opening 26 acts as a resistance obstructing the flow of the gaseous target X2.
- the resistance is too large, and the flow rate of the gaseous target X2 decreases, and when the diameter D2 of the other end of the opening 26 is greater than 5 mm, the resistance is too small and the flow rate of the gaseous target X2 increases excessively.
- the ionizer 40 can be made in a state suitable for ionizing the target by beam irradiation.
- a length L of the opening 26 along the flow of the sample droplet X1 may be 0.5 mm to 100 mm. Similar to the diameter D2 of the other end of the opening 26, the length L of the opening 26 along the flow of the sample droplet X1 acts as a resistance to obstruct the flow of the gaseous target X2. If the length L of the opening 26 along the flow of the sample droplet X1 is smaller than 0.5 mm, the flow rate of the gaseous target X2 may increase, causing turbulence or lowering detection sensitivity. If the length L of the opening 26 along the flow of is greater than 100 mm, the flow rate of the gaseous target X2 may decrease, resulting in low detection sensitivity.
- the set temperature of the block 24 may be 50 °C to 500 °C. If the temperature of the block 24 is lower than 50°C, the sample may not evaporate, and if the temperature of the block 24 is higher than 500°C, the molecular structure of the target may be broken.
- the diameter D1 of one end of the aperture 26, the diameter D2 of the other end of the aperture 26, the length L of the aperture 26 along the flow of the sample droplet X1, and the temperature of the block 24 Accordingly, the state of the target supplied to the mass spectrometer 50 is changed. Since the state of the target required by the mass spectrometer 50 varies depending on the type of target, the diameter D1 of one end of the aperture 26, the diameter D2 of the other end of the aperture 26, and the diameter of the sample droplet X1 By controlling the length L of the opening 26 along the flow and the temperature of the block 24, various types of targets can be analyzed with one mass spectrometer 50.
- the block 24 includes a plurality of pieces (24a, 24b, 24c), a plurality of pieces (24a, 24b, 24c) are coupled to each other to form one block (24) form.
- the first, second, and third pieces 24a, 24b, and 24c include elements constituting at least one opening 26, and when the first, second, and third pieces 24a, 24b, and 24c are combined, the elements are also combined to form a complete opening 26 .
- the first piece 24a includes the inclined surface 28 of the opening 26, and the second and third pieces 24b and 24c include portions of the opening 26 having a constant diameter. Accordingly, when the first, second, and third pieces 24a, 24b, and 24c are combined, at least one complete opening 26 is formed.
- Block 24 according to another example makes it possible to easily adjust the length (L) of the opening 26 according to the type of target. That is, if a plurality of pieces 24a, 24b, and 24c having different specifications (eg, slope, diameter, length, etc.) are prepared, necessary pieces may be assembled and used according to the type of target. Therefore, it is not necessary to manufacture a plurality of blocks 24 according to the type of target.
- the inlet tube 30 is disposed downstream of the evaporator 20 and connects the evaporator 20 , the ionizer 40 , and the mass spectrometer 50 to each other.
- the inlet tube 30 includes first, second and third conduits 32, 34 and 36.
- the first conduit 32 includes both ends, and one end is connected to the evaporator 20, that is, the second part 22b of the housing 22, so that the gaseous target X2 evaporated by the block 24 is the first conduit 32. It is introduced into the inlet tube 30 through the conduit 32.
- the second conduit 34 includes both ends, one end connected to the ionizer 40 and the other end connected to the other end of the first conduit 32 . Accordingly, the beam X3 (eg, helium beam) generated by the ionizer 40 is irradiated to the gaseous target X2 flowing through the first and third conduits 32 and 36 to ionize the target.
- a means for preventing the inflow of the gaseous target X2 and irradiating the beam X3 to the gaseous target X2 may be mounted at the other end of the second conduit 34 .
- the third conduit 36 includes both ends, one end connected to the other ends of the first and second conduits 32 and 34 and the other end connected to the mass spectrometer 50 .
- the gaseous target X2 introduced into the inlet pipe 30 through the first conduit 32 passes through the junctions of the first, second, and third conduits 32, 34, and 36, and is irradiated with a beam to be ionized. It is supplied to the mass spectrometer 50 through the three conduits 36.
- the ionizer 40 generates a beam X3 and irradiates it to the gaseous target X2 flowing through the first and third conduits 32 and 36 through the second conduit 34. By this, at least the target included in the gaseous target X2 is ionized.
- the ionizer 40 may be a DART and the beam X3 generated by the ionizer 40 may be a helium beam.
- the DART as the ionizer 40, it is possible to ionize non-polar low-molecular-weight materials or silicon-based compounds that are difficult to ionize with other ionization methods. Since the ionizer 40, particularly the DART, is well known to those skilled in the art, further detailed descriptions thereof are omitted.
- the mass spectrometer 50 is connected to the other end of the third conduit 36 to receive and analyze a sample containing an ionized target. Accordingly, the mass spectrometer 50 may output a mass spectrum of the target. Since the mass spectrometer 50 is well known to those skilled in the art, further detailed description is omitted.
- FIG. 4 is a flowchart of a sample analysis method according to another embodiment of the present invention.
- step S100 by liquid chromatography (5), liquid chromatography is performed to separate and elute a sample containing a target of a single component.
- the sample separated and eluted by the liquid chromatography (5) is converted into a sample droplet (X1) by the droplet atomizer (10), and is converted into a sample droplet (X1) through the probe (12) through the evaporator (20). It is injected into (S110).
- the droplet atomizer 10 may be an electric atomizer or a gas atomizer. In addition, sheath gas may additionally be used.
- the sample droplet X1 injected into the evaporator 20 passes through at least one opening 26 in the block 24 heated to a set temperature and is evaporated to become a gaseous target X2 (S120).
- a gaseous target X2 S120
- an inclined surface 28 is formed at one end of each opening 26 facing the droplet sprayer 10 so that as many sample droplets X1 sprayed from the droplet sprayer 10 enter the opening 26 as possible. can do.
- appropriate specifications may be mounted on the housing 22 prior to the analysis of the target.
- the gaseous target X2 evaporated by block 24 is introduced into the first conduit 32 of the inlet tube 30 and travels toward the mass spectrometer 50.
- the ionizer 40 irradiates the beam X3 to the gaseous target X2 through the second conduit 34 to ionize the target included in the gaseous target X2 (S130).
- the ionizer 40 may be a DART
- the beam X3 generated by the ionizer 40 may be a helium beam.
- step S140 the ionized target is introduced into the mass spectrometer 50 through the third conduit 36, and mass spectrometry is performed.
- Example 5 is a diagram showing the molecular structure of a material according to Example 1.
- Example 1 a material having a molecular structure shown in FIG. 5 was analyzed using a liquid chromatography mass spectrometer according to an embodiment of the present invention.
- an electric atomizer was used as the droplet atomizer 10
- a sheath gas was additionally used for effective solvent evaporation
- a DART irradiating a helium beam was used as the ionizer 40.
- the elemental composition of the material according to Example 1 is C6H3BrFI and the exact mass is 299.8.
- Example 6 is a mass spectrum of a material according to Example 1 by a liquid chromatography mass spectrometer according to an embodiment of the present invention.
- a mass spectrum of the material according to Example 1 could not be obtained using a conventional liquid chromatography mass spectrometer using APCI as an ionizer.
- APCI liquid chromatography mass spectrometer
- DART liquid chromatography mass spectrometer
- a clear mass spectrum of the material according to Example 1 could be obtained (see FIG. 6).
- the mass-to-charge ratio (m/z) was found to be 316.8.
- FIG. 7 is a view showing the molecular structure of a material according to Example 2
- FIG. 8 is a view showing the molecular structure of a material according to Example 3.
- Examples 2 and 3 materials having molecular structures shown in FIGS. 7 and 8 were analyzed using a liquid chromatography mass spectrometer according to an embodiment of the present invention.
- an electric atomizer was used as the droplet atomizer 10
- a sheath gas was additionally used for effective solvent evaporation
- a DART irradiating a helium beam was used as the ionizer 40.
- the exact mass of the material according to Example 2 is 1224.1
- the exact mass of the material according to Example 3 is 1410.2.
- FIG. 9 is a mass spectrum of a material according to Example 2 by a liquid chromatography mass spectrometer according to an embodiment of the present invention
- FIG. 10 is a mass spectrum of a material according to Example 2 by a liquid chromatography mass spectrometer according to the prior art
- 11 is a mass spectrum of a material according to Example 3 by a liquid chromatography mass spectrometer according to an embodiment of the present invention
- FIG. 12 is a mass spectrum according to Example 3 by a liquid chromatography mass spectrometer according to the prior art. is the mass spectrum of a substance.
- Mass spectra of the materials according to Examples 2 and 3 using a conventional liquid chromatography mass spectrometer using APCI as an ionizer showed peaks at various mass-to-charge ratios (m/z) (see FIGS. 10 and 12).
- m/z mass-to-charge ratios
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Abstract
Description
Claims (15)
- 액체 크로마토그래피(Liquid Chromatography; LC), 이온화 장치, 그리고 질량 분석기(Mass Spectrometer; MS)의 인터페이스에 있어서,상기 액체 크로마토그래피에서 용출된 표적을 포함하는 시료는 이온화 장치에 의하여 이온화되어 질량 분석기로 도입되고,상기 인터페이스는액체 크로마토그래피에서 용출된 표적을 포함하는 시료를 시료 액적의 형태로 변환하여 분사하는 액적 분무기;상기 표적을 질량 분석기로 도입하는 도입관; 그리고상기 액적 분무기와 도입관 사이에 배치되어 시료 액적에 포함된 용매를 증발시켜 가스상 표적을 생성하는 증발기;를 포함하며,상기 이온화 장치는 도입관 내의 가스상 표적에 빔을 조사하여 도입관을 통해 질량 분석기로 도입되는 상기 가스상 표적을 이온화시키고,상기 증발기는 적어도 하나의 개구가 형성되고 가열될 수 있는 블록을 포함하며,상기 액적 분무기에서 분사된 시료 액적은 상기 적어도 하나의 개구를 통과하며 가스상 표적으로 생성되고, 생성된 가스상 표적이 도입관으로 흘러가는 인터페이스.
- 제1항에 있어서,상기 적어도 하나의 개구의 액적 분무기를 향하는 일단부는 시료 액적의 흐름을 따라 그 직경이 줄어드는 경사면으로 형성되는 인터페이스.
- 제1항에 있어서,상기 적어도 하나의 개구의 직경 또는 길이는 조절 가능한 인터페이스.
- 제1항에 있어서,상기 블록은 복수의 조각을 포함하며, 상기 복수의 조각이 서로 결합되어 하나의 블록을 형성하는 인테페이스.
- 제4항에 있어서,상기 증발기는 하우징을 더 포함하고,상기 블록은 상기 시료 액적의 흐름에 교차하도록 상기 하우징 내에 탈착 가능하게 장착되는 인터페이스.
- 제2항에 있어서,상기 개구의 일단의 직경은 1mm ~ 20mm이고, 상기 개구의 타단의 직경은 0.1mm ~ 5mm이며, 시료 액적의 흐름을 따른 개구의 길이는 0.5mm ~ 100mm인 인터페이스.
- 제1항에 있어서,상기 블록은 설정된 온도로 가열되며,상기 설정된 온도는 50℃ ~ 500℃인 인터페이스.
- 제1항에 있어서,상기 이온화 장치는 헬륨 빔을 조사하는 DART인 인터페이스.
- 액체 크로마토그래피에 의하여, 액체 크로마토그래피를 수행하여 단일 성분의 표적을 포함하는 시료를 분리 및 용출하는 단계;액적 분무기에 의하여, 액체 크로마토그래피로부터 용출된 표적을 포함하는 시료를 시료 액적의 형태로 변환하여 분사하는 단계;증발기에 의하여, 액적 분무기로부터 분사된 시료 액적 내의 용매를 증발시켜 가스상 표적을 생성하는 단계;이온화 장치에 의하여, 가스상 표적에 빔을 조사하여 가스상 표적을 이온화하는 단계; 그리고질량 분석기에 의하여, 이온화된 표적의 질량 분석을 수행하는 단계;를 포함하는 시료 분석 방법.
- 제9항에 있어서,증발기는 하우징과, 시료 액적의 흐름에 교차하도록 상기 하우징 내에 탈착 가능하게 장착되고 설정된 온도로 가열될 수 있는 블록을 포함하는 시료 분석 방법.
- 제10항에 있어서,상기 블록은 적어도 하나의 개구를 포함하며,액적 분무기에 의하여 분사된 시료 액적은 적어도 하나의 개구를 통과하며 가스상 표적으로 생성되고, 생성된 가스상 표적은 도입관을 통하여 질량 분석기로 도입되는 시료 분석 방법.
- 제11항에 있어서,상기 적어도 하나의 개구의 상기 액적 분무기를 향하는 일단부는 시료 액적의 흐름을 따라 그 직경이 줄어드는 경사면으로 형성되는 시료 분석 방법.
- 제11항에 있어서,이온화 장치는 상기 도입관 내에서 흐르는 가스상 표적에 헬륨 빔을 조사하는 DART인 시료 분석 방법.
- 제10항에 있어서,표적에 따라 개구의 직경 또는 길이, 또는 설정된 온도를 조정하는 단계를 더 포함하는 시료 분석 방법.
- 제14항에 있어서,상기 개구의 일단의 직경은 1mm ~ 20mm이고, 상기 개구의 타단의 직경은 0.1mm ~ 5mm이며, 시료 액적의 흐름을 따른 개구의 길이는 0.5mm ~ 100mm이고, 설정된 온도는 50℃ ~ 500℃인 시료 분석 방법.
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US18/036,476 US20230400439A1 (en) | 2021-07-20 | 2022-07-20 | Interface Between Liquid Chromatography, Ionization Device, and Mass Spectrometer, and Sample Analysis Method Using the Same |
EP22846205.7A EP4215913A4 (en) | 2021-07-20 | 2022-07-20 | INTERFACE BETWEEN LIQUID CHROMATOGRAPHY, IONIZATION DEVICE AND MASS SPECTROMETER AND SAMPLE ANALYSIS METHODS THEREFOR |
JP2023528489A JP2023549819A (ja) | 2021-07-20 | 2022-07-20 | 液体クロマトグラフィー、イオン化装置、及び質量分析器の間のインターフェースおよびそれを用いた試料分析方法 |
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JP2013007639A (ja) * | 2011-06-24 | 2013-01-10 | Hitachi High-Technologies Corp | 液体クロマトグラフ質量分析装置 |
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