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WO2009110026A1 - Procédé de spectrométrie de masse et spectroscope de masse - Google Patents

Procédé de spectrométrie de masse et spectroscope de masse Download PDF

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Publication number
WO2009110026A1
WO2009110026A1 PCT/JP2008/000452 JP2008000452W WO2009110026A1 WO 2009110026 A1 WO2009110026 A1 WO 2009110026A1 JP 2008000452 W JP2008000452 W JP 2008000452W WO 2009110026 A1 WO2009110026 A1 WO 2009110026A1
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mass
signal
ion
ions
autocorrelation function
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English (en)
Japanese (ja)
Inventor
西口克
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Shimadzu Corp
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Shimadzu Corp
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/025—Detectors specially adapted to particle spectrometers
    • H01J49/027—Detectors specially adapted to particle spectrometers detecting image current induced by the movement of charged particles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes
    • H01J49/34—Dynamic spectrometers
    • H01J49/40—Time-of-flight spectrometers
    • H01J49/408—Time-of-flight spectrometers with multiple changes of direction, e.g. by using electric or magnetic sectors, closed-loop time-of-flight

Definitions

  • the present invention relates to a mass spectrometric method and a mass spectroscope, and more particularly to a mass spectrometric method and a mass spectroscope using an ion optical system that separates ions according to mass by flying ions along a circular orbit.
  • time-of-flight mass spectrometers measure the flight time required for ions to fly a certain distance based on the principle that ions accelerated with a constant energy have a flight speed according to the mass. The mass of the ion is calculated. Therefore, it is effective to increase the flight distance in order to improve the mass resolution.
  • a multi-round time-of-flight mass spectrometry that achieves high mass resolution by extending the flight distance of ions by increasing the number of rounds using a multi-round ion optical system that makes multiple rounds of ions along a closed orbit Devices have been developed (see Patent Documents 1, 2, and 3, Non-Patent Document 1, etc.).
  • a multi-reflection time-of-flight mass spectrometer using a multi-reflection ion optical system has been developed that extends the flight distance by reflecting ions several times with a reflection electric field.
  • the multi-round time-of-flight mass spectrometer can achieve a high mass resolution
  • the drawback is that as the ions circulate, ions that fly faster due to the smaller mass overtake slower ions on a closed orbit due to the larger mass.
  • peaks having different laps, that is, having different flight distances are mixed on the spectrum. In that case, since the mass of the ion and the flight distance cannot be uniquely determined, the mass spectrum cannot be obtained directly from the time-of-flight spectrum.
  • a multi-turn time-of-flight mass spectrometer is generally used to observe only a narrow mass range in which no overtaking occurs among ions generated by an ion source.
  • Patent Document 4 One technique for solving this problem is proposed in Patent Document 4.
  • a plurality of different time-of-flight spectra are obtained by performing a plurality of measurements while changing the time from the incidence to the exit of ions to the orbit.
  • These time-of-flight spectra include peaks for ions of the same mass that have different lap times. Therefore, by calculating the multiple correlation function of the plurality of time-of-flight spectra, the time-of-flight spectrum of a single revolution is reconstructed and converted into a mass spectrum.
  • a detector capable of detecting passing ions electromagnetically and non-destructively (maintaining ions as they are) on a periodic orbit by a multi-circular ion optical system is installed, and a signal for a predetermined period of time is installed.
  • the detection signal includes a plurality of periodic signals having a frequency depending on the mass of ions. This signal can be converted into a frequency spectrum by Fourier transform, and the frequency spectrum can be easily converted into a mass spectrum from the correspondence between the frequency and the mass. Thereby, the target mass spectrum can be obtained by subjecting the detection signal acquired by only one measurement to Fourier transform.
  • This method can be said to be an excellent mass spectrometry method for avoiding the problems of the multi-round time-of-flight mass spectrometer.
  • this method will be referred to as “Fourier Transform Multiple Loop Mass Spectrometry (FT-MT / MS)”.
  • FT / MS mass spectrometry
  • FT-ICR / MS Fourier transform ion cyclotron resonance mass spectrometry
  • Non-Patent Document 2 An apparatus for reciprocating ions in an electrostatic field of a specific shape and performing mass spectrometry using the frequency has been developed.
  • FT-MT / MS is an excellent method for avoiding the problems of the multi-round time-of-flight mass spectrometer, but has one problem compared to other FT / MS. It is a problem related to the signal observation time required to obtain a predetermined mass resolution. The problem will be described below.
  • the mass resolution obtained depends on the frequency resolution of the apparatus.
  • the signal observation time required for obtaining a predetermined frequency resolution depends on the frequency of ion motion included in the signal.
  • f is the frequency of motion for ions of mass m
  • ⁇ f is the frequency peak width.
  • ⁇ is a constant depending on the device, and is 1 for FT-ICR / MS and 0.5 for FT-MT / MS.
  • FIG. 5 shows the relationship between the mass m and the motion frequency f for each of FT-MT / MS and FT-ICR / MS, which is obtained by the equations (5) and (7).
  • FT-MT / MS requires a signal observation time that is one to two digits longer than other FT / MS (specifically, FT-ICR / MS) to achieve the same mass resolution. Therefore, the measurement throughput is significantly reduced. This is one problem in FT-MT / MS.
  • One of the causes of the above problems lies in the characteristics of signal analysis by Fourier transform, in which the width of the frequency peak by Fourier transform depends on the signal observation time.
  • FT-MT / MS when the signal observation time is extended, that is, when the number of laps is increased, ion packets (a set of ions taking into account the spread in the time direction) of two types of ions close to each other in mass are separated.
  • the characteristics of Fourier transform even if the ion packets are separated, the frequency corresponding to the two ion packets cannot be separated on the frequency spectrum unless sufficient signal observation time is taken. That is, although the signal observation time is extended to improve the spatial separation, the improvement in the separation does not necessarily lead to the improvement in mass resolution.
  • JP 11-1335060 A Japanese Patent Application Laid-Open No. 11-135031 JP 11-195398 A JP 2005-79049 A JP-A-2005-79037 M. Toyoda and three others, “Multi-turn time-of-flight mass spectrometers with electrostatic sectors”, Journal of ⁇ Mass Spectrometry (J. Mass Spectrom.), 38, pp. 1125-1142, 2003 Marshall (AGMarshall) and two others, “Fourier Transform Ion Cyclotron Resonance Mass Spectrometry: Fourier Transform Ion Cyclotron Resonance Mass Spectrometry: A Mass Spectrom. Rev.), 17, pp.1-35, 1998
  • the present invention has been made to solve the above-described problems.
  • a mass spectrometer that combines a multi-circular ion optical system and an ion non-destructive detector
  • the problems of conventional signal analysis by Fourier transform are solved.
  • the main purpose is to overcome and achieve high resolution and high throughput (or high speed).
  • the mass spectrometric method according to the present invention which has been made to solve the above-mentioned problems, spatially separates ions derived from a sample according to the mass by repeatedly flying ions derived from a sample along a circular orbital orbit.
  • a mass spectrometric method using a mass spectroscope comprising a multi-circular ion optical system and a detection means for non-destructively detecting ions flying on the circular orbit or reciprocating orbit,
  • ACF Auto-Correlation Function
  • a mass spectrometer made to solve the above problems is an apparatus for carrying out the mass spectrometry method according to the present invention, a) a multi-circular ion optical system that spatially separates ions according to mass by repeatedly flying ions derived from a sample along a circular or reciprocating orbit; b) non-destructive detection means for detecting ions flying on the orbit or reciprocating orbit, c) an arithmetic processing means for extracting a periodicity of the observed signal and calculating a periodic spectrum by calculating an autocorrelation function for the observed signal obtained within a predetermined signal observation time by the detecting means; d) conversion processing means for calculating the mass spectrum or the mass of each ion from the periodic spectrum; It is characterized by having.
  • the signal observed by the detection means from when the ions are emitted from the ion source arranged outside the multi-circular ion optical system until the predetermined signal observation time elapses indicates information on the ions passing therethrough. Includes all. That is, every time an ion having a certain mass makes a round orbit (or travels one way along the reciprocating orbit), a peak for that ion should appear, and this peak has a period corresponding to the mass. When a plurality of types of ions having different masses are mixed, the peaks having the periodicity as described above are mixed or sometimes overlapped. In the present invention, signal analysis is performed on such an observation signal using an autocorrelation function instead of Fourier transform.
  • the autocorrelation function is a function that indicates how much an observed signal at a certain time is correlated with a signal after a certain period of time has elapsed. Therefore, by finding a signal having a high autocorrelation, it is possible to extract the periodicity of the peak according to the mass of the various ions described above.
  • an autocorrelation function C () defined by the following equation (9) with respect to an observation signal f (t) (0 ⁇ t ⁇ S) obtained within the signal observation time S: ⁇ ) (0 ⁇ ⁇ ⁇ S) can be used. Also, since the denominator of equation (9) is not important, only the numerator of the following equation can be used.
  • the peak width appearing in the autocorrelation function is twice the peak width in the original time domain and does not depend on the signal observation time in terms of the calculation principle.
  • the width of the frequency peak by the Fourier transform used in the conventional FT-MT / MS depends on the signal observation time even in terms of the calculation principle. Therefore, in the mass spectrometry method and the mass spectrometer according to the present invention, the signal observation time is extended with respect to two ion packets having close masses, and at least the ion packets are separated in space. There is a possibility that the respective masses can be calculated by separating the periods corresponding to the ion packets.
  • the period for two types of ions that are separated on the observation signal cannot be separated by simply performing processing using the autocorrelation function. This is a case where the masses of the two types of ions are very close and separation can be confirmed on the observation signal only after many rounds. Therefore, in order to improve the resolution of the period for ions separated on the observation signal, in the present invention, for example, the following arithmetic processing is preferably performed on the autocorrelation function of the observation signal.
  • the autocorrelation function product F (T) may be obtained from the following equation (10) for the result obtained in the autocorrelation function.
  • W (n T ) is a weight function, and a predetermined function with 1 or n T as a variable can be used.
  • [x] represents a maximum integer not exceeding x.
  • the autocorrelation function product directly represents the signal intensity with respect to the flight period of the multi-turn ion optical system, that is, the periodic spectrum.
  • the acceleration voltage of ions is constant, the cycle of one round depends on the mass of ions. Therefore, the periodic spectrum based on the autocorrelation function product is substantially equivalent to the mass spectrum, and the mass can be easily calculated.
  • the signal observation time is shorter than that of the conventional FT-MT / MS by about two digits or three digits, which is sufficiently high to meet the extended flight distance. Mass resolution can be obtained. Further, multiple rounds of measurement need only be performed once, and it is not necessary to repeat the measurement for the same sample many times as in the case of MT / MS using a conventional multiple correlation function. Accordingly, the total measurement time can be shortened, and samples need only be prepared as much as necessary for one measurement.
  • FIG. 1 It is a schematic block diagram of the mass spectrometer by one Example of this invention, (A) is an example using a multiple circulation ion optical system, (B) is an example using a multiple reflection ion optical system.
  • a multi-circular ion optical system is designed to have a first-order or higher time convergence point with respect to the initial position of ions, the incident angle of ions, and the energy of ions.
  • the time width of the ion packet after going around 100 laps that is, the temporal spread of the same type of ions, is on the order of several tens [ns] at the time convergence point. It is.
  • the period when the ions make one round is approximately on the order of several to several tens [ ⁇ s] under a common-sense acceleration voltage condition. Therefore, if the ion non-destructive detector is ideal and the passage time width of the ion packet can be accurately observed, the ion passage signal observed for the circular motion of one kind of ion is: A peak having a width of about 10 to several tens [ns] is a periodic signal that appears every 10 to several tens [ ⁇ s].
  • FIG. 6 is a schematic diagram showing the state of an observation signal for a single type of ion.
  • an autocorrelation function of the ion passage signal f (t) is calculated.
  • the denominator is a constant factor introduced by definition and is not important for the purpose here.
  • A is a constant. From this, the following two items can be confirmed. (1) In the autocorrelation function, a peak is obtained with respect to a period T included in the signal with respect to an integer multiple of the period not exceeding the signal observation time. (2) The peak width appearing in the autocorrelation function is twice the peak width observed in the original signal.
  • the above (1) is that the autocorrelation function has the property of extracting the periodicity included in the signal, and the observed signal is correlated with the time delay of iT (1 ⁇ i ⁇ n ⁇ 1) due to its property. It is due to that there is.
  • (2) shows that the peak width of the autocorrelation function depends only on the peak width of the observation signal. This is a significant feature in contrast to the fact that the frequency peak width in Fourier transform depends on the signal observation time.
  • the physical meaning of this result is only that the periodicity of 2nT and 2nT + 2 ⁇ T exists in the observed signal f (t) with a width of 2 ⁇ T, respectively, and exists in the original signal f (t).
  • the periods T and T + ⁇ T / n can not be analyzed.
  • the ultimate purpose is to analyze the periodicity of T and T + ⁇ T / n included in the observation signal f (t) with the shortest signal observation time possible. Therefore, further ingenuity is required to increase the periodic resolution.
  • the multiple product given by the above equation (10) is calculated for the autocorrelation function.
  • this is an operation for taking a geometric mean for all values of an integer multiple period that can be observed.
  • the reliability and accuracy of the determination are improved.
  • the autocorrelation function product it is possible to increase the influence of the determination of the autocorrelation function at the maximum number of rotations showing the highest resolution.
  • the signal observation time required to obtain a predetermined resolution is about twice that when a multi-turn ion optical system is used as a time-of-flight mass spectrometer. This is because the peak width of the autocorrelation function is twice the peak width of the observation signal. This signal observation time is much shorter than the value required for the conventional FT / MS as described above.
  • a general multi-turn time-of-flight mass spectrometer requires several hundred rounds in order to achieve a mass resolution of 100,000, and the flight time required is on the order of several to several tens [ms]. Therefore, also in the mass spectrometer according to the present invention, the required flight time is on the order of 10 to 100 [ms].
  • the signal observation time required by the present invention is a value that is about 1 to 2 digits smaller.
  • the mass spectrometry method and the mass spectrometer according to the present invention overcome the problems of the conventional FT-MT / MS with respect to the signal observation time required to achieve a predetermined mass resolution, and Compared with FT / MS, it provides an advantage in terms of signal observation time. Specifically, in the present invention, measurement with almost the same resolution is possible with a signal observation time shorter by one to two digits than other FT / MS, and the measurement throughput is greatly improved. .
  • FIG. 1 is a schematic configuration diagram of a mass spectrometer according to the present embodiment, where (A) is an example using a multi-circular ion optical system, and (B) is an example using a multiple reflection ion optical system.
  • the mass spectrometer shown in FIG. 1 (A) gives an initial kinetic energy to various ions and outputs them all at once, that is, an ion source 1 that starts flight, a plurality of electrodes (not shown), and voltages to the electrodes.
  • a multi-circular ion optical system 3 that repeatedly flies ions along the same circular orbit 6 by the action of a plurality of electric fields formed by electrodes, and an incident orbit 5 emitted from the ion source 1.
  • the ion incident switch 2 for introducing ions traveling along the circular orbit 6 by the multi-circular ion optical system 3 and the number (quantity) of ions passing along the circular orbit 6 of the multi-circular ion optical system 3 and passing therethrough.
  • a signal processing unit 7 that receives the detection signal from the detector 4 and executes the arithmetic processing as described above.
  • the ion injection switch 2 is an orbital deflection element that can be driven in a pulsed manner. While the ion incident switch 2 is on, the ion trajectory is deflected so that ions are introduced from the incident trajectory 5 to the circular orbit 6, and when the switch 2 is off, it can be considered that the switch 2 is not present.
  • the flying ions pass through the switch 2 as they are.
  • the detector 4 can output an electrical signal corresponding to the passage amount of ions that are charged particles by using, for example, electromagnetic induction.
  • the number of ion packets having different periods (that is, masses), the mass of each ion, and the ion intensity are generated by random numbers, and these ion packets are emitted from the ion source 1 and repeated on the orbit 6.
  • a simulation calculation was performed on the ion passage signal obtained by the detector 4 when it was made to fly.
  • the length Lin of the incident orbit 5 is 0.6 [m]
  • the length L of one turn of the circular orbit 6 is 1.0 [m].
  • the distribution of ion packets is an ideal Gaussian distribution, and the ion acceleration voltage is 10 [kV].
  • the detector 4 is ideal so that the passing signal can be accurately observed without any loss of ions.
  • the sampling rate of the ion passage signal is 1 [GHz].
  • the simulation result of the ion passage signal at this time is shown in FIG.
  • the signal observation time is 0 to 100 [ ⁇ s].
  • the mass range that can be introduced into the circular orbit 6 is limited by the size of the apparatus due to its structure.
  • Ions ejected in a pulse form from the ion source 1 at a constant acceleration voltage are introduced into the orbit 6 through the incident trajectory 5 and the ion incident switch 2.
  • the ions simultaneously emitted from the ion source 1 also vary spatially according to the mass before reaching the ion injection switch 2. Therefore, while the ion injection switch 2 is kept on in order to introduce ions having a low speed into the orbit 6, the ions introduced earlier at a higher speed orbit the orbit 6 and reach the ion injection switch 2 again. A situation can occur.
  • the cycle period T i of the ion packet is from the ion source 1 to the detector 4.
  • T i (L / L ′) t i
  • Automatic peak detection is easy. Therefore, based on the flight time of each peak observed within the time range, all of the values that can exist as the cycle of the ion packet introduced into the orbit 6 are defined by the observed peak width. It is possible to calculate within an error range in advance, that is, before calculating an autocorrelation function or the like as described later. Specifically, it can be calculated using a time-of-flight spectrum in a time range of 0 ⁇ t ⁇ t f obtained when ions pass through the detector 4 for the first time.
  • FIG. 3A shows a periodic spectrum obtained by calculating the autocorrelation function product for the observation signal after performing the preliminary period determination as described above for the observation signal shown in FIG.
  • the weighting function W (n T ) is 1.
  • FIG. 3B shows a periodic spectrum corresponding to the number and mass of ion packets generated by random numbers. In the periodic spectrum by the autocorrelation function product shown in FIG. 3A, it can be confirmed that all the generated periods are calculated without omission.
  • FIG. 4 shows the calculation result. It can be seen that the mass identification result obtained from the autocorrelation function product agrees very well with the original data generated. Thereby, it has confirmed that high mass identification accuracy was realizable with the mass spectrometry method and mass spectrometer which concern on this invention.
  • the ions pass through the detector 4 on the forward path and the return path of the reciprocating orbit 6 '. Therefore, the length L of one turn of the orbit 6 corresponds to the reciprocal distance from passing through the detector 4 to passing through the detector 4 in the opposite direction again, as shown in FIG.
  • the length of one round trip of the inner round trip track 6 ′ is 2L.
  • the peak positions that is, the periods are in good agreement, but the relative relationship of the intensity of each peak changes. Since the peak intensity does not affect the qualitative property at all, there is no problem when performing qualitative analysis by mass identification. On the other hand, when quantitative accuracy is required, it is necessary to improve the reproducibility of the peak intensity.
  • the resolution of the periodic spectrum has been improved by calculating the multiple product of the autocorrelation function, but in order to achieve the same effect, another method such as harmonic averaging should be used. You can also.

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Abstract

Selon l'invention, sur une orbite de révolution (6) constituée d'un système optique d'ions multiples tournants (3), est disposé un détecteur (4) qui est capable de détecter d'une manière non destructive l'ion qui le traverse. Le détecteur (4) acquiert un signal pour observer une période allant de l'émission d'ion à partir d'une source ionique (1) jusqu'à l'expiration d'un temps d'observation de signal donné, et une section de processeur de signal (7) calcule de multiples produits pour une fonction d'autocorrélation d'un tel signal afin de déterminer un spectre périodique extrayant les cycles propres à chaque ion. Etant donné que la masse et le cycle de révolution correspondent entre eux, un spectre de masse est obtenu à partir d'un spectre périodique. La largeur de crête d'un cycle qui est déterminée par la fonction d'autocorrélation est indépendante du temps d'observation de signal si bien qu'il est possible d'assurer la séparabilité d'une crête de cycle sans augmenter le temps d'observation de signal. De plus, le calcul de produits de la fonction d'autocorrélation permet également de séparer sur le spectre périodique deux crêtes du signal qui ne sont séparées qu'au moment de l'augmentation du nombre de révolutions, séparées aussi sur le spectre périodique, la résolution en masse étant ainsi améliorée.
PCT/JP2008/000452 2008-03-05 2008-03-05 Procédé de spectrométrie de masse et spectroscope de masse Ceased WO2009110026A1 (fr)

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JP2011198624A (ja) * 2010-03-19 2011-10-06 Shimadzu Corp 質量分析データ処理方法及び質量分析装置
JP2012122761A (ja) * 2010-12-06 2012-06-28 Mitsubishi Rayon Co Ltd 重合体の測定方法
CN102939638A (zh) * 2010-03-02 2013-02-20 莱克公司 开口阱质谱仪
JP2022069775A (ja) * 2020-10-26 2022-05-12 日本電子株式会社 マススペクトル処理装置及び方法

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CN102939638A (zh) * 2010-03-02 2013-02-20 莱克公司 开口阱质谱仪
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JP2016006795A (ja) * 2010-03-02 2016-01-14 レコ コーポレイションＬｅｃｏ Ｃｏｒｐｏｒａｔｉｏｎ オープントラップ質量分析計
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JP2022069775A (ja) * 2020-10-26 2022-05-12 日本電子株式会社 マススペクトル処理装置及び方法
JP7249980B2 (ja) 2020-10-26 2023-03-31 日本電子株式会社 マススペクトル処理装置及び方法
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