WO2018029847A1 - Dispositif chromatographique, procédé d'analyse chromatographique, programme d'analyse chromatographique et base de données d'analyse chromatographique - Google Patents

Dispositif chromatographique, procédé d'analyse chromatographique, programme d'analyse chromatographique et base de données d'analyse chromatographique Download PDF

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WO2018029847A1
WO2018029847A1 PCT/JP2016/073729 JP2016073729W WO2018029847A1 WO 2018029847 A1 WO2018029847 A1 WO 2018029847A1 JP 2016073729 W JP2016073729 W JP 2016073729W WO 2018029847 A1 WO2018029847 A1 WO 2018029847A1
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sample
measurement
quantitative value
chromatograph
target compound
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PCT/JP2016/073729
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English (en)
Japanese (ja)
Inventor
雄紀 坂本
崇史 住吉
雄太郎 山村
道一 稲葉
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株式会社島津製作所
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Priority to PCT/JP2016/073729 priority Critical patent/WO2018029847A1/fr
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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
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/483—Physical analysis of biological material
    • G01N33/487—Physical analysis of biological material of liquid biological material
    • G01N33/49—Blood
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor

Definitions

  • the present invention relates to a chromatograph apparatus, a chromatographic analysis method, and a chromatographic analysis program used for separating and quantifying a compound contained in a sample from other compounds, such as a gas chromatograph and a liquid chromatograph.
  • the present invention also relates to a chromatographic analysis database that can be suitably used in quantitative analysis using a chromatographic apparatus.
  • a detector such as a mass spectrometer or an absorptiometer.
  • a device using a mass spectrometer as a detector is called a chromatograph mass spectrometer.
  • MRM multiple reaction monitoring
  • SIM selected ion monitoring
  • samples When performing MRM measurement or SIM measurement of a plurality of specimens (samples), it is common to set the plurality of samples in an autosampler and sequentially introduce them into a chromatograph mass spectrometer for continuous measurement. is there.
  • the sample may remain in the vaporization chamber (in the case of a gas chromatograph) or a flow path of an autosampler or chromatograph, and may be mixed (carry over) in the next sample.
  • a carry-over occurs, a quantitative value larger than the actual quantitative value of the target compound contained in the next sample is obtained.
  • MRM measurement and SIM measurement are used, for example, when quantifying drugs contained in biological samples and pesticides contained in food samples.
  • the quantification results are determined by laws and regulations regarding the content of drugs and pesticides in samples. It is used to determine whether or not the specified reference value is exceeded. Therefore, if the quantitative value of the target compound contained in the sample is larger than the actual quantitative value of the target compound due to carryover, and the result exceeds the standard value, it is erroneously determined that the law is violated.
  • a blank sample that does not include the target compound for example, a sample that includes only a mobile phase of a chromatograph or a solvent
  • Measures are taken in the same manner as the actual sample and then the next actual sample is measured.
  • the chromatograph mass spectrometer is described as an example, but there is a problem similar to the above when a detector such as an absorptiometer is used.
  • the problem to be solved by the present invention is to perform continuous measurement efficiently while preventing the occurrence of erroneous measurement results due to carryover when continuously measuring the target compound contained in each of a plurality of samples.
  • a chromatograph apparatus, a chromatographic analysis method, and a chromatographic analysis program are provided.
  • the database for chromatographic analysis which can be used suitably when performing the said continuous measurement in a chromatograph apparatus is provided.
  • a first aspect of the present invention made to solve the above problems is a chromatographic apparatus for measuring a common target compound contained in a plurality of samples, a) a chromatograph section having a column for temporally separating the compound contained in the sample, and a detector for measuring the compound separated by the column; b) a storage unit storing calibration information in which the measurement intensity of the target compound in the detector is associated with the quantitative value of the target compound; c) a quantitative value calculating unit for obtaining a quantitative value of the target compound contained in the sample based on the calibration information each time measurement of one sample is completed in the chromatograph unit; d) a determination unit for determining whether or not the quantitative value obtained by the quantitative value calculation unit exceeds a predetermined threshold; and e) introducing a plurality of preset samples one by one into the chromatograph unit.
  • the predetermined threshold value is determined based on, for example, the ratio of the target compound mixed into the next sample due to carry-over and the lower limit of detection or the lower limit of quantification of the target compound determined based on the result of preliminary measurement. Can do. That is, when carryover occurs during measurement of a sample, a quantitative value at which the amount of the target compound mixed in the sample to be measured next reaches the detection lower limit value or the lower limit of quantification can be used as the threshold value. In addition, in order to distinguish from the 2nd threshold value mentioned later, this threshold value is suitably called “the 1st threshold value" in this specification.
  • the target compound contained in the sample is quantified at the end of measurement of each sample, and it is determined whether or not the quantified value exceeds a threshold value.
  • a threshold value since only a real sample is continuously measured as long as the quantitative value does not exceed the threshold, continuous measurement can be performed more efficiently than in the past.
  • the introduction of the next sample is suspended, so the quantitative measurement is performed in a state where the target compound contained in the previous sample is mixed into the next sample to be measured. Can be prevented.
  • g) When the determination unit determines that the quantitative value exceeds the threshold value, a blank sample that does not contain the target compound is introduced into the chromatograph unit, or a blank sample is introduced without introducing any sample.
  • a configuration may be provided that includes a blank measurement execution unit that performs measurement.
  • Performing measurement without introducing any sample means that the target compound is measured in a state where only the mobile phase is allowed to flow when using a liquid chromatograph, for example.
  • the mobile phase not only a solution having a single composition but also a mobile phase for gradient analysis, which is a mixed solution of a plurality of solutions and the mixing ratio changes with time, can be used.
  • the target compound contained in the sample measured previously is discharged from the chromatograph and prevented from affecting the sample to be measured next. Can do.
  • the quantitative value calculation unit calculates the quantitative value of the target compound from the result of the blank measurement,
  • the determination unit determines whether the quantitative value of the target compound in the blank measurement exceeds a predetermined second threshold; When the determination unit determines that the quantitative value of the target compound in the blank measurement exceeds the second threshold, the blank measurement execution unit performs the blank measurement again, and otherwise
  • the sample introduction unit can be configured to resume the introduction of the plurality of samples.
  • the detection lower limit value or the quantification lower limit value of the target compound described above can be suitably used.
  • higher / lower values may be used depending on the required measurement accuracy. For example, even if the quantitative value of the target compound at the time of blank measurement is above the lower limit of quantification, if the carry-over in the next analysis can be reliably predicted to fall below the lower limit of quantification, the second threshold value is used. A value higher than the lower limit of quantification can be set.
  • the actual sample measured immediately before contains a large amount of the target compound. Even if the target compound remaining in the blank measurement is discharged, the measurement of the next sample is still affected. If the target compound remains in an amount that may be affected (for example, an amount corresponding to the lower limit of detection or lower limit of quantification of the target compound), blank measurement is performed again to discharge the target compound. Thereby, since the amount of the target component mixed in the sample to be measured next is reduced to substantially zero, it is possible to reliably prevent the target compound from being quantified in error. In addition, after the blank measurement, if there is no residual target compound in an amount that affects the measurement of the next sample, the measurement of the actual sample is automatically resumed. Measurements can be made.
  • a second aspect of the present invention made to solve the above problems is a chromatograph comprising a column for temporally separating a compound contained in a sample, and a detector for measuring the compound separated by the column.
  • a method for measuring a common target compound contained in a plurality of samples a) introducing one of the plurality of samples into the chromatograph; b) Obtaining a quantitative value of the target compound based on the result of measuring the introduced sample with the detector and calibration information of the target compound prepared in advance, c) determine whether the quantitative value exceeds a predetermined threshold; d) When the quantitative value does not exceed the threshold value, the next sample is introduced into the chromatograph, and when the quantitative value exceeds the threshold value, introduction of the sample into the chromatograph is suspended. The measurement is interrupted.
  • the third aspect of the present invention made to solve the above problems is a chromatographic analysis program for causing a computer to execute the method.
  • the fourth aspect of the present invention is a database used in the chromatographic apparatus of the first aspect, wherein each of the plurality of compounds is a) one or more sets of measurement parameters used to measure each of the compounds; b) calibration information associated with each of the one or more sets of measurement parameters and used to quantify the compound from the measurement result of the compound; c) It is characterized in that, in the continuous measurement of a plurality of samples, each time a measurement of one sample is completed, a reference value used for determining whether or not a blank measurement is necessary is associated.
  • the principal part block diagram of the liquid chromatograph mass spectrometer which is one Example of the chromatograph apparatus which concerns on this invention.
  • the flowchart of one Example of the chromatographic analysis method which concerns on this invention. 1 is an example of a chromatographic analysis database according to the present invention. Analysis condition setting screen in the present embodiment.
  • FIG. 1 is a configuration diagram of a main part of a liquid chromatograph mass spectrometer of the present embodiment
  • FIG. 2 is a flowchart relating to the chromatographic analysis method of the present embodiment
  • FIG. 3 is a chromatographic analysis database of the present embodiment.
  • the liquid chromatograph mass spectrometer of the present embodiment is roughly composed of a liquid chromatograph 1 and a control unit 4 for controlling the operation thereof.
  • the liquid chromatograph 1 includes a mobile phase container 10 in which a mobile phase is stored, a pump 11 that sucks the mobile phase and feeds it at a constant flow rate, an injector 12 that injects a predetermined amount of sample liquid into the mobile phase, And a column 13 for separating various compounds contained in the sample solution in the time direction, and a mass spectrometer 2 as a detector for measuring the compounds separated by the column 13. Further, the liquid chromatograph 1 is connected to an autosampler 14 for introducing a plurality of liquid samples into the injector 12 one by one.
  • the mass spectrometer 2 includes a first vacuum chamber whose degree of vacuum is increased stepwise between an ionization chamber 20 that is substantially atmospheric pressure and a high vacuum analysis chamber 23 that is evacuated by a vacuum pump (not shown). 2 A multi-stage differential exhaust system having intermediate vacuum chambers 21 and 22 is provided.
  • the ionization chamber 20 is provided with an electrospray ionization probe (ESI probe) 201 for spraying while applying a charge to the sample solution.
  • ESI probe electrospray ionization probe
  • the ionization chamber 20 and the first intermediate vacuum chamber 21 in the subsequent stage communicate with each other through a small heating capillary 202.
  • the first intermediate vacuum chamber 21 and the second intermediate vacuum chamber 22 are separated by a skimmer 212 having a small hole at the top, and ions are focused in the first intermediate vacuum chamber 21 and the second intermediate vacuum chamber 22, respectively.
  • ion guides 211 and 221 for transporting to the subsequent stage are installed.
  • the analysis chamber 23 sandwiches a collision cell 232 in which a multipole ion guide (q2) 233 is installed, and the former quadrupole mass filter (Q1) 231 that separates ions according to the mass-to-charge ratio, A quadrupole mass filter (Q3) 234 and an ion detector 235 are installed to separate the two according to the mass-to-charge ratio.
  • CID gas such as argon or nitrogen is appropriately supplied in accordance with the measurement conditions.
  • the mass spectrometer 2 can perform SIM (selected ion monitoring) measurement, MS / MS scan measurement (product ion scan measurement), MRM (multiple reaction monitoring) measurement, and the like.
  • SIM selected ion monitoring
  • MS / MS scan measurement product ion scan measurement
  • MRM multiple reaction monitoring
  • ions are not sorted by the front quadrupole mass filter (Q1) 231 (not functioning as a mass filter), and the mass-to-charge ratio of ions passing through the rear quadrupole mass filter (Q3) 234 is fixed.
  • Q1 front quadrupole mass filter
  • Q3 mass-to-charge ratio of ions passing through the rear quadrupole mass filter
  • both the front quadrupole mass filter (Q1) 231 and the rear quadrupole mass filter (Q3) 234 are caused to function as mass filters.
  • the first-stage quadrupole mass filter (Q1) 231 passes only ions set as precursor ions. Further, CID gas is supplied into the collision cell 232, and the precursor ions are cleaved to generate product ions.
  • the mass-to-charge ratio of ions passing through the subsequent quadrupole mass filter (Q3) 234 is scanned.
  • the mass-to-charge ratio of ions passing through the subsequent quadrupole mass filter (Q3) 234 is scanned. Fix it.
  • the control unit 4 includes a storage unit 41, and includes a measurement control unit 42, a quantitative value calculation unit 43, a determination unit 44, and a blank measurement execution unit 45 as functional blocks.
  • the entity of the control unit 4 is a personal computer, and the CPU of the personal computer functions as each of the above units by executing a chromatographic analysis program installed in advance in the computer.
  • An input unit 6 and a display unit 7 are connected to the control unit 4.
  • the storage unit 41 stores in advance a chromatographic analysis database in which analysis conditions for a plurality of known compounds are described.
  • the chromatographic analysis database includes measurement conditions, calibration information, reference values (first threshold value in the present invention) used for determining whether or not the first blank measurement needs to be performed, and blank measurement re-execution.
  • the lower limit of quantification (second threshold in the present invention) used for determining whether or not is necessary is associated with each other.
  • the chromatographic analysis database is stored in a table format as shown in FIG. 3, for example.
  • Measurement conditions include column type, retention time, MRM transition (a combination of the precursor ion and product ion mass-to-charge ratio selected during MRM measurement), collision energy (energy for cleaving the precursor ion during MRM measurement), etc. include.
  • the calibration information is information in which the mass-to-charge ratio of ions derived from each compound and the measurement intensity of the ions having the mass-to-charge ratio are associated with the compound concentration, and is stored in a mathematical expression or a table format.
  • the reference value is a value that serves as a reference for determining whether or not there is a possibility of an error in the quantitative value of the target compound related to the sample to be measured next due to carry-over from the sample measured previously. Specifically, from the carryover ratio of the target compound determined by preliminary measurement or the like (the ratio of the target compound remaining in the sample previously measured) and the lower limit of quantification (or lower limit of detection) of the target compound. Desired.
  • the reference value when the carryover is 0.1% and the lower limit of quantification is 1 ng / ml is 1000 ng / ml.
  • the configuration is such that the lower limit of quantification and the reference value are stored in the database, but the ratio of the lower limit of quantification and the carryover may be stored, and the reference value may be obtained from them.
  • the measurement control unit 42 instructs the user to analyze conditions (measurement conditions). , Calibration information, and reference value) are displayed on the display unit 7.
  • An example of the analysis condition input screen is shown in FIG.
  • the target compound, the column to be used, and the MRM transition are selected from the analysis conditions by pull-down in this order.
  • column 1 and column 2 can be selected in the column column. If column 1 is selected here, the retention time is automatically determined, and three types of MRM transitions can be selected.
  • the CE value and calibration information are automatically determined, and the corresponding lower limit of quantification and reference value are read and displayed.
  • the lower limit of quantification is a specified value, but the displayed value may be used as it is for the reference value or may be changed.
  • the measurement control unit 42 After determining the analysis conditions, when the user performs a predetermined operation (for example, by pressing the “analysis start” button displayed on the screen), the measurement control unit 42 sets the measurement target sample set in the autosampler 14. Analysis (quantification of compound A contained in each sample) is started.
  • the measurement control unit 42 operates the autosampler 14 to inject the sample 1 from the injector 12 and measures the compound A based on the analysis conditions determined by the above procedure. That is, from the ions generated from the compound introduced from the column 13 to the ESI probe 201, ions having a mass-to-charge ratio of 200 are selected as precursor ions by the front quadrupole mass filter 231, and a collision energy of 5.0 V is applied thereto. Apply and cleave at collision cell 232. Then, product ions having a mass-to-charge ratio of 125 are selected from the generated product ions by the subsequent quadrupole mass filter 234 and measured by the ion detector 235 (step S2).
  • ions of the same MRM transition may be always measured during measurement of the sample.
  • the MRM transition is switched in accordance with their retention times. Measurement signals from the ion detector 235 are sequentially sent to the control unit 4 and stored in the storage unit 41.
  • the quantitative value calculation unit 43 reads the measurement signal of the compound A related to the sample 1 from the storage unit 41, obtains the measurement intensity, creates a mass chromatogram, and displays it on the display unit 7. Further, the intensity of the peak located at the retention time of Compound A in the mass chromatogram is determined. This intensity varies depending on whether the calibration curve information is based on the peak top intensity or the peak area. Based on the peak intensity and the calibration curve information, a quantitative value of compound A contained in sample 1 is obtained (step S3). The quantitative value is displayed on the display unit 7.
  • the determination unit 44 determines whether or not the quantitative value obtained by the quantitative value calculation unit 43 is less than the reference value (step S4). If the quantitative value is less than the reference value (YES in step S4), it is determined whether there is a sample to be measured next. Here, since samples 2 to 100 have not been measured, it is determined that there is a sample to be measured next (YES in step S5), and the process returns to step S2 to measure the next sample (sample 2). The samples 2 to 100 are sequentially measured in the same manner as described above. When it is determined that there is no sample to be measured next (NO in step S5), the measurement ends.
  • the introduction of the actual sample by the autosampler 14 is temporarily stopped and the continuous measurement is interrupted.
  • the display unit 7 displays that the continuous measurement is interrupted.
  • the blank measurement execution unit 45 operates the autosampler 14 to introduce a blank sample into the injector 12.
  • the reason why the measurement of the actual sample is interrupted and the blank sample is introduced is to prevent an error in the quantitative value of the next sample when the compound A carries over from the previously measured sample. . If Compound A remains in the sample collection section in the autosampler 14, the injector 12, or the flow path from the autosampler 14 to the column 13, it will be mixed into the sample to be measured next. For example, if the previously measured sample contains Compound A at a concentration of 1000 ng / ml, and 0.1% of that is carried over, the next sample will be mixed with Compound A at a concentration of 1 ng / ml. This concentration corresponds to the lower limit of quantification of Compound A, and causes an error in the quantification value of Compound A contained in the next sample.
  • the solvent of Compound A is used as a blank sample.
  • a mobile phase, a cleaning solution, or the like can be used as long as Compound A can be discharged from the flow path or the like.
  • a mobile phase for gradient measurement which is a mixed solution of a plurality of types of solvents and changes the mixing ratio with time, can also be used.
  • the measurement of the compound A contained in the blank sample is performed in the same manner as the measurement target sample described above.
  • Compound A is not contained in the blank sample itself, but in the blank measurement, compound A carried over from the previous sample is discharged and measured.
  • Measurement signals from the ion detector 235 are sequentially stored in the storage unit 41.
  • the quantitative value calculation unit 43 reads the measurement signal of the compound A from the storage unit 41 for the blank sample, obtains the measurement intensity, creates a mass chromatogram, and displays it on the display unit 7. Further, the intensity of the peak located at the retention time of Compound A in the mass chromatogram is determined. Based on the peak intensity and calibration curve information, a quantitative value of compound A contained in sample 1 is obtained (step S7). Further, the quantitative value is displayed on the display unit 7.
  • the sample measured earlier contains 1000 ng / ml or more of Compound A.
  • the quantitative value of Compound A in the blank measurement is 1 ng / ml (the lower limit of quantification of Compound A). That's it.
  • the determination unit 44 also determines whether the value of the quantitative value of Compound A obtained for the blank sample is less than the lower limit of quantification of Compound A. If the quantitative value is less than the quantitative lower limit value (YES in step S8), it is determined whether there is a sample to be measured next. If there is a sample to be measured next (NO in step S5), the process returns to step S2 to measure the next sample (sample 2), and if there is no sample to be measured next (NO in step S5). A series of measurement operations is completed. As described above, in this example, since the next sample is measured after confirming that the quantitative value of Compound A is below the lower limit of quantification at the time of blank measurement, the compound A mixed in the sample to be measured next is measured. Compound A can be correctly quantified with the amount reduced to substantially zero.
  • the blank measurement execution unit 45 operates the autosampler 14 and introduces the blank sample into the injector 12 again. Compound A is measured. The introduction and measurement of the blank sample are repeated until the quantitative value of Compound A is less than the lower limit of quantification (YES in Step S8).
  • the above-described embodiment is an example, and can be appropriately changed in accordance with the gist of the present invention.
  • values higher / lower than these may be set according to the accuracy required for measurement, and stored in the chromatographic analysis database in advance. For example, even if the quantitative value of the target compound at the time of blank measurement exceeds the lower limit of quantification, if it can be reliably predicted that the carryover in the next analysis will be lower than the lower limit of quantification, the lower limit of quantification is not necessarily set as the threshold value.
  • the threshold value higher than the lower limit of quantification can be set as appropriate.
  • the reference value can be appropriately changed according to the required measurement accuracy.
  • the chromatographic detector is not limited to a mass spectrometer.
  • an absorptiometer, a fluorescence detector, a differential refractive index detector, an evaporative light scattering detector, etc. can be used.
  • a thermal conductivity type detection is possible.
  • a detector, a hydrogen flame ionization detector, an electron capture detector, a flame photometric detector, or the like can be used.
  • the measurement conditions and calibration information in the chromatographic analysis database are appropriately created according to the detector to be used.

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Abstract

La présente invention concerne un dispositif chromatographique destiné à mesurer un composé cible commun inclus dans une pluralité d'échantillons qui est pourvu : d'une unité de chromatographie 1 ayant une colonne 13 pour séparer temporellement les composés inclus dans un échantillon et un détecteur 2 pour mesurer les composés séparés par la colonne 13 ; une unité de stockage 41 dans laquelle sont stockées des informations d'étalonnage dans lesquelles des intensités de mesure de composés cibles sont associées à des valeurs quantitatives ; une unité de calcul de valeurs quantitatives 43 pour, à chaque fois que l'unité de chromatographie 1 achève la mesure d'un échantillon, déterminer une valeur quantitative pour le composé cible inclus dans l'échantillon sur la base des informations d'étalonnage ; une unité de détermination 44 pour déterminer si la valeur quantitative déterminée dépasse un seuil prédéterminé ; une unité d'introduction d'échantillons 14 pour introduire une pluralité d'échantillons qui ont été définis à l'avance dans l'unité de chromatographie 1 un par un ; et une unité de commande de mesure 42 pour arrêter l'introduction d'échantillons par l'unité d'introduction d'échantillons 14 et interrompre la mesure lorsque l'unité de détermination 44 détermine que la valeur quantitative dépasse le seuil.
PCT/JP2016/073729 2016-08-12 2016-08-12 Dispositif chromatographique, procédé d'analyse chromatographique, programme d'analyse chromatographique et base de données d'analyse chromatographique WO2018029847A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114609257A (zh) * 2020-12-08 2022-06-10 中国科学院大连化学物理研究所 一种气相色谱质谱仪及其气路控制方法
WO2023054125A1 (fr) * 2021-10-01 2023-04-06 株式会社日立ハイテク Procédé de commande pour dispositif de spectrométrie de masse de chromatographe en phase liquide

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JP2011237462A (ja) * 2007-02-01 2011-11-24 Sysmex Corp 検体分析装置

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JPH10318803A (ja) * 1997-05-21 1998-12-04 Shimadzu Corp 分析装置
JP2011237462A (ja) * 2007-02-01 2011-11-24 Sysmex Corp 検体分析装置

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114609257A (zh) * 2020-12-08 2022-06-10 中国科学院大连化学物理研究所 一种气相色谱质谱仪及其气路控制方法
CN114609257B (zh) * 2020-12-08 2023-04-25 中国科学院大连化学物理研究所 一种气相色谱质谱仪及其气路控制方法
WO2023054125A1 (fr) * 2021-10-01 2023-04-06 株式会社日立ハイテク Procédé de commande pour dispositif de spectrométrie de masse de chromatographe en phase liquide

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