US20170276652A1 - Analyzing device - Google Patents
Analyzing device Download PDFInfo
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- US20170276652A1 US20170276652A1 US15/506,820 US201415506820A US2017276652A1 US 20170276652 A1 US20170276652 A1 US 20170276652A1 US 201415506820 A US201415506820 A US 201415506820A US 2017276652 A1 US2017276652 A1 US 2017276652A1
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- flow passage
- pressure
- flow
- supercritical fluid
- analyzing
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/36—Control of physical parameters of the fluid carrier in high pressure liquid systems
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/40—Selective adsorption, e.g. chromatography characterised by the separation mechanism using supercritical fluid as mobile phase or eluent
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/14—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
-
- 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
- G01N30/86—Signal analysis
- G01N30/8651—Recording, data aquisition, archiving and storage
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06G—ANALOGUE COMPUTERS
- G06G7/00—Devices in which the computing operation is performed by varying electric or magnetic quantities
- G06G7/48—Analogue computers for specific processes, systems or devices, e.g. simulators
- G06G7/75—Analogue computers for specific processes, systems or devices, e.g. simulators for component analysis, e.g. of mixtures, of colours
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/328—Control of physical parameters of the fluid carrier of pressure or speed valves, e.g. check valves of pumps
-
- 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
- G01N30/80—Fraction collectors
Definitions
- the present invention relates to an analyzing device that separates a plurality of components contained in a sample into the individual components, and specifically, relates to a chromatograph using supercritical fluid.
- Supercritical fluid can be realized by holding fluid that is gas at normal temperature and normal pressure (for example, carbon dioxide) at higher temperature and pressure than those at the critical point of the fluid (in the case of carbon dioxide, the critical temperature is 31° C. and the critical pressure is 7.4 MPa).
- the supercritical fluid exhibits excellent ability as solvent to many substances, and is often used for supercritical fluid extraction (hereinafter referred to as SFE) and supercritical fluid chromatography (hereinafter referred to as SFC).
- Patent Literature 1 discloses an extraction and separation/analyzing device using supercritical fluid which can perform any of SFE and SFC by switching between a flow system for SFE and a flow system for SFC with a switching valve.
- a component extracted from a sample by SFE is first trapped in a trap column, and then, is eluted with a solvent. Therefore, in order to measure the SFE-extracted substances by the chromatograph, human intervention is needed for adjusting the concentration of the extracted substance and placing it in a sample introducing unit of the chromatograph.
- an off-line configuration in which extracted substances are not directly introduced into a column, a series of operations from extraction to analysis cannot be automatically performed.
- Patent Literature 2 discloses an analyzing device using supercritical fluid which has an on-line configuration in which SFE and SFC are integrated into one flow system, and is capable of automatically performing a series of operations from extraction to analysis.
- An example of such an analyzing device with the on-line configuration is shown in FIG. 3 .
- the analyzing device 30 of FIG. 3 is configured of a cylinder 300 , a pressurizing pump 301 , a solvent container 302 , a modifier pump 303 , a first flow passage switching valve 304 , a sample storing container 305 , a temperature adjusting device 306 , a needle 307 , a second flow passage switching valve 308 , an analyzing column 309 , an ultraviolet detector (UV) 310 , a back pressure regulating valve 311 and a mass spectrometer (MS) 312 .
- UV ultraviolet detector
- MS mass spectrometer
- Carbon dioxide that is drawn out of the cylinder 300 by the pressurizing pump 301 and pressurized (to supercritical fluid) is sent, via the first flow passage switching valve 304 along with a modifier agent drawn out of the solvent container 302 , to the sample storing container 305 which is temperature controllable by the temperature adjusting device 306 .
- the pressurizing pump 301 and the later-mentioned back pressure regulating valve 311 the pressure of the flow passage between them is set to a pressure exceeding the critical pressure, and the temperature of the sample storing container 305 is set to a temperature exceeding the critical temperature by the temperature adjusting device 306 .
- carbon dioxide is put into supercritical state inside the sample storing container 305 , and the supercritical carbon dioxide, with its excellent capability as solvent, extract components from a sample in the sample storing container 305 (SFE).
- the supercritical fluid containing the SFE-extracted components flows into the analyzing column 309 from the needle 307 attached to the sample storing container 305 via the second flow passage switching valve 308 .
- the supercritical fluid containing the SFE-extracted components is separated to individual components by the analyzing column 309 , and then, flows through the ultraviolet detector (UV) 310 , the back pressure regulating valve 311 and the mass spectrometer (MS) 312 , where the individual components are analyzed (SFC).
- UV ultraviolet detector
- MS mass spectrometer
- the conventional analyzing device 30 When an agricultural product is analyzed as a sample by a chromatograph to measure the amount of pesticide residues in the agricultural product using the conventional analyzing device 30 , a large amount of substances that constitute noise to the analysis of the pesticide, such as pigments, lipids and saccharides in the agricultural product itself, are extracted in addition to the target component in the SFE-extracted components.
- the configuration of the conventional analyzing device 30 when such a sample is analyzed, the entirety of the SFE-extracted components is introduced into the analyzing column 309 . Consequently, the analyzing column 309 tends to deteriorate due to the large amount of unwanted constituents, and saturation of the ultraviolet detector (UV) 310 and contamination of the mass spectrometer (MS) 312 tend to arise.
- the analyzing device 30 may be burdened or correct measurement may be difficult, which narrows the range of analyzable samples of the analyzing device 30 and lessens its versatility.
- a problem to be solved by the present invention is to provide a highly versatile analyzing device that widens the range of analyzable samples.
- An analyzing device devised to solve the aforementioned problem includes:
- a splitting part for causing fluid containing a sample component to flow separately in a first flow passage and a second flow passage
- flow rate of the fluid in the first flow passage and flow rate of the fluid in the second flow passage are controlled based on a ratio of the pressure in the first flow passage to the pressure in the second flow passage.
- an analyzing method according to the present invention devised to solve the aforementioned problem includes the steps of:
- the “fluid” is preferably supercritical fluid, but it is not limited to this, and it may be gas or liquid.
- the pressure in the first flow passage and the pressure in the second flow passage are set such that a sum of values of these pressures is a value of a pressure exceeding a critical pressure of the fluid.
- Both of the first pressure controlling unit and the second pressure controlling unit may have pressure controlling valves, and the pressure controlling valves may be provided on the first flow passage and the second flow passage respectively.
- an extracting unit (SFE Unit) for performing extraction using supercritical fluid (SFE) may be connected, or a sample injecting unit (auto-sampler) may be connected.
- SFE Unit extracting unit for performing extraction using supercritical fluid
- auto-sampler sample injecting unit
- the analyzing device and the analyzing method according to the present invention having the aforementioned configurations, by changing the ratio of the pressure in the first flow passage to the pressure in the second flow passage using the first pressure controlling unit and the second pressure controlling unit, the flow rate of the fluid in the first flow passage and flow rate of the fluid in the second flow passage after split at the splitting part can be controlled.
- the flow rate of the fluid in the column provided on the first flow passage is reduced such that the entirety of the unwanted constituents is not introduced into the column. This can suppress deterioration of the column and can reduce burden on the analyzing device. In this way, a highly versatile analyzing device that can widen the range of analyzable samples can be provided.
- FIG. 1 is a schematic configuration diagram of an analyzing device according to a first embodiment of the present invention.
- FIG. 2 is a schematic configuration diagram of an analyzing device according to a second embodiment of the present invention.
- FIG. 3 is a schematic configuration diagram of a conventional analyzing device.
- FIG. 1 is a schematic configuration diagram of an analyzing device of a first embodiment.
- the analyzing device 10 of this embodiment is configured of a cylinder 100 , a pressurizing pump 101 , a solvent container 102 , a modifier pump 103 , an extracting unit 114 , an analyzing column 109 , a splitting part 110 , a first back pressure regulating valve 111 , a second back pressure regulating valve 112 , a mass spectrometer (MS) 113 and a recovering container 115 .
- the extracting unit 114 is configured of a first flow passage switching valve 104 , a sample storing container 105 , a temperature adjusting device 106 , a needle 107 , a second flow passage switching valve 108 , and pipes connecting these.
- the analyzing device 10 of this embodiment has a feature of including the splitting part 110 , the first back pressure regulating valve 111 and the second back pressure regulating valve 112 .
- Fluid containing sample components flows in pipes separately in two flow passages of a first flow passage and a second flow passage by means of the splitting part 110 .
- This embodiment has an on-line configuration in which the extracting unit 114 is directly connected upstream of the splitting part 110 , and the analyzing column 109 is directly connected to the first flow passage downstream thereof
- description will be made to a case where the extracting unit 114 extracts pesticide residues contained in a sample (agricultural product) by SFE using carbon dioxide as supercritical fluid, and the analyzing column 109 separates components in the pesticide residues.
- the first back pressure regulating valve 111 and the second back pressure regulating valve 112 that are pressure controlling valves correspond to a first pressure controlling unit and a second pressure controlling unit, respectively.
- the analyzing device 10 operates as follows to separate a plurality of components contained in extracted substances by the extracting unit 114 into the individual components using the analyzing column 109 , thereby to identify the individual components by the mass spectrometer 113 .
- an agricultural product as a sample is put in the sample storing container 105 , to one end of which the needle 107 is attached.
- These operations may be performed by a user or may be performed by a not-shown controlling device. In this way, the individual parts are connected as in FIG. 1 .
- One or plurality of sample storing container s 105 may be prepared as in FIG. 1 , and a configuration may be adopted in which extraction for a plurality of samples can be performed.
- carbon dioxide (supercritical fluid) is drawn out of the cylinder 100 under pressurization by the pressurizing pump 101 .
- a modifier agent that is a polar solvent (methanol, ethanol or the like) is drawn out of the solvent container 102 by the modifier pump 103 .
- These are sent, via the first flow passage switching valve 104 , to the sample storing container 105 which is temperature controllable by the temperature adjusting device 106 such as a heater.
- the pressure in a flow passage between the pressurizing pump 101 and the splitting part 110 is set to be a pressure exceeding the critical pressure (7.4 MPa) of carbon dioxide by the pressurizing pump 101 and the later-mentioned first back pressure regulating valve 111 and second back pressure regulating valve 112 , and the sample storing container 105 is set to have a temperature exceeding the critical temperature (31° C.) of carbon dioxide by the temperature adjusting device 106 , carbon dioxide is in the supercritical state (supercritical fluid) inside the sample storing container 105 . Since carbon dioxide in the supercritical state exhibits excellent ability as solvent, it dissolves the sample (agricultural product) in the sample storing container 105 . Thereby, in addition to pesticide residues that are the target components in the sample, a large amount of substances that constitute noise to analysis of the pesticide residues, such as pigments, lipids and saccharides, are extracted (SFE).
- the supercritical fluid containing the SFE-extracted components reaches the splitting part 110 from the needle 107 via the second flow passage switching valve 108 , and splits thereat into the first flow passage and the second flow passage.
- the analyzing column 109 heated at a temperature exceeding the critical temperature by a not-shown column oven is provided on the first flow passage, and thus the supercritical fluid containing the SFE-extracted components and flowing in the first flow passage is in the supercritical state inside the analyzing column 109 .
- the supercritical fluid flows in the first back pressure regulating valve 111 and the mass spectrometer (MS) 113 , where the individual components are analyzed (SFC).
- a detector (ultraviolet detector (UV) 310 or the like) (not shown) may be provided between the analyzing column 109 and the first back pressure regulating valve 111 , and the mass spectrometer 113 is not essential. After the supercritical fluid containing the SFE-extracted components and flowing in the second flow passage is released from the supercritical state by flowing in the second back pressure regulating valve 112 , it is recovered by the recovering container 115 .
- UV ultraviolet detector
- the pressure in the first flow passage controlled by the first back pressure regulating valve 111 is P 1
- the pressure in the second flow passage controlled by the second back pressure regulating valve 112 is P 2
- the resistance of the analyzing column 109 is eliminated for convenience of description.
- the values of the pressures P 1 and P 2 which realize a desired split ratio can be grasped by investigating relation between the ratio of the pressures P 1 to P 2 and the flow rate in advance thorough a preliminary experiment.
- the sum of the values of the pressure P 1 in the first flow passage and the pressure P 2 in the second flow passage should be set to be the value of a pressure exceeding the critical pressure of the fluid.
- the flow rate of the fluid in the first flow passage and the flow rate of the fluid in the second flow passage after split at the splitting part 110 can be controlled.
- the flow rate of the fluid in the analyzing column 109 provided on the first constitute noise to the is reduced as in the aforementioned example of the split ratio 1:99 in order to prevent the entirety of the fluid from being introduced into the analysing column 109 .
- the flow rate of the fluid in the analyzing column 109 can be changed by changing the ratio of the pressure P 1 in the first flow passage to the pressure P 2 in the second flow passage. Therefore, in the case of employing the configuration in which the extracting unit 114 for performing extraction using supercritical fluid (SFE) is provided upstream of the splitting part 110 , the flow rate in the analyzing column 109 provided on the first flow passage can be reduced while the flow rate in the sample storing container 105 in the extracting unit 114 is increased, which can realize the flow rates respectively suitable for SFE and SFC. Thereby, in an on-line configuration in which SFE and SFC are integrated into one flow system, accurate analysis in which the sample components are sufficiently separated in the analyzing column 109 and broad peaks are reduced is possible.
- SFE supercritical fluid
- the portion can be subjected to subsequent analysis using another analyzing device as in the case of an off-line configuration.
- first back pressure regulating valve 111 and the second back pressure regulating valve 112 correspond to the first pressure controlling unit and the second pressure controlling unit, respectively, and have the same piping structures, it is not limited to this, and a mechanism in which structures (sectional shapes and sizes of sectional areas) of pipes constituting the first flow passage and the second flow passage are different from each other may be used for the first pressure controlling unit and the second pressure controlling unit.
- FIG. 2 is a schematic configuration diagram of an analyzing device of a second embodiment.
- the analyzing device 20 of this embodiment includes a third flow passage switching valve 21 and an autosampler 22 in addition to the similar configuration to that of the analyzing device 10 of the first embodiment including the cylinder 100 , the pressurizing pump 101 , the solvent container 102 , the modifier pump 103 , the extracting unit 114 , the analyzing column 109 , the splitting part 110 , the first back pressure regulating valve 111 , the second back pressure regulating valve 112 , the mass spectrometer (MS) 113 and the recovering container 115 .
- MS mass spectrometer
- the third flow passage switching valve 21 is connected upstream of the splitting part 110 , and the splitting part 110 is connected to the extracting unit 114 or the autosampler 22 by changing connections between ports in the valve 21 as shown in dotted lines or solid lines.
- the autosampler 22 corresponds to a sample injecting unit.
- a configuration in which the splitting part 110 is connected to is the same with that in the first embodiment, and hereafter, description will be made to a configuration in which the splitting part 110 is connected to the autosampler 22 and only chromatography (SFC) using supercritical fluid can be performed.
- carbon dioxide (supercritical fluid) is drawn out of the cylinder 100 .
- a modifier agent that is a polar solvent (methanol, ethanol or the like) is drawn out of the solvent container 102 by the modifier pump 103 .
- They are sent to the autosampler 22 as a mobile phase (fluid) through the third flow passage switching valve 21 provided between the pressurizing pump 101 and the modifier pump 103 , and the first flow passage switching valve 104 , and a sample is injected in the autosampler 22 .
- the sample injected by the autosampler 22 reaches the splitting part 110 again via the third flow passage switching valve 21 on a flow of the mobile phase.
- the mobile phase containing the sample is supplied to the splitting part 110 . Then, after the components are separated into individual components in the analyzing column 109 similarly to the first embodiment, the mobile phase flows in the first back pressure regulating valve 111 and the mass spectrometer (MS) 113 , where the individual components are analyzed (SFC). Also in this embodiment, a detector (ultraviolet detector (UV) 310 or the like) (not shown) may be provided between the analyzing column 109 and the first back pressure regulating valve 111 , and the mass spectrometer 113 is not an essential configuration.
- a detector ultraviolet detector (UV) 310 or the like
- a user can freely select and use the on-line configuration in which SFE and SFC are integrated into one flow system or the configuration in which only chromatography (SFC) using supercritical fluid can be performed by changing the connections between the ports in the third flow passage switching valve 21 . Therefore, a sample is not limited to one in the state before performing SFE, which can widen the range of analysable samples more than conventional and can enhance versatility of an analyzing device.
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Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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PCT/JP2014/072533 WO2016031008A1 (ja) | 2014-08-28 | 2014-08-28 | 分析装置 |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/JP2014/072533 A-371-Of-International WO2016031008A1 (ja) | 2014-08-28 | 2014-08-28 | 分析装置 |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US17/672,482 Division US20220170892A1 (en) | 2014-08-28 | 2022-02-15 | Analyzing device |
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US20170276652A1 true US20170276652A1 (en) | 2017-09-28 |
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US15/506,820 Abandoned US20170276652A1 (en) | 2014-08-28 | 2014-08-28 | Analyzing device |
US17/672,482 Pending US20220170892A1 (en) | 2014-08-28 | 2022-02-15 | Analyzing device |
Family Applications After (1)
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US17/672,482 Pending US20220170892A1 (en) | 2014-08-28 | 2022-02-15 | Analyzing device |
Country Status (4)
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US (2) | US20170276652A1 (ja) |
JP (1) | JP6265268B2 (ja) |
CN (1) | CN106662554B (ja) |
WO (1) | WO2016031008A1 (ja) |
Cited By (6)
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EP3657163A1 (en) * | 2018-11-22 | 2020-05-27 | Shimadzu Corporation | Analysis assistance method, analysis assistance device, analysis assistance program and analysis system |
US20210231622A1 (en) * | 2018-06-07 | 2021-07-29 | Shimadzu Corporation | Method of measuring accuracy of concentration in sending liquid in gradient and liquid chromatograph having function of executing method |
EP3779432A4 (en) * | 2018-04-13 | 2022-01-05 | Shimadzu Corporation | EXTRACT RECOVERY PROCESS AND ANALYSIS PROCESS |
US11243193B2 (en) | 2017-02-13 | 2022-02-08 | Shimadzu Corporation | Supercritical fluid device |
JP2022097535A (ja) * | 2018-11-22 | 2022-06-30 | 株式会社島津製作所 | 分析支援方法および分析支援装置 |
EP3896440A4 (en) * | 2018-12-10 | 2022-08-17 | Hitachi High-Tech Corporation | LIQUID CHROMATOGRAPHY MASS SPECTROMETER |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110243951A (zh) * | 2018-03-09 | 2019-09-17 | 株式会社岛津制作所 | 超临界流体萃取仪与液质联用仪的连接装置 |
CN113874723B (zh) * | 2019-06-11 | 2023-09-22 | 株式会社岛津制作所 | 超临界流体装置用流动相调温装置及超临界流体装置 |
JP7468845B2 (ja) | 2020-07-27 | 2024-04-16 | 株式会社島津製作所 | 分析支援装置、分析支援方法、分析支援プログラムおよび分析システム |
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2014
- 2014-08-28 CN CN201480081635.7A patent/CN106662554B/zh active Active
- 2014-08-28 US US15/506,820 patent/US20170276652A1/en not_active Abandoned
- 2014-08-28 WO PCT/JP2014/072533 patent/WO2016031008A1/ja active Application Filing
- 2014-08-28 JP JP2016545156A patent/JP6265268B2/ja active Active
-
2022
- 2022-02-15 US US17/672,482 patent/US20220170892A1/en active Pending
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Also Published As
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CN106662554B (zh) | 2019-04-02 |
JPWO2016031008A1 (ja) | 2017-04-27 |
JP6265268B2 (ja) | 2018-01-24 |
WO2016031008A1 (ja) | 2016-03-03 |
US20220170892A1 (en) | 2022-06-02 |
CN106662554A (zh) | 2017-05-10 |
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