CN210294180U - Full two-dimensional gas chromatography and Fourier transform ion cyclotron resonance mass spectrum coupling system - Google Patents
Full two-dimensional gas chromatography and Fourier transform ion cyclotron resonance mass spectrum coupling system Download PDFInfo
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Abstract
The utility model provides a full two-dimensional gas chromatography and Fourier transform ion cyclotron resonance mass spectrum coupled system, this coupled system includes full two-dimensional gas chromatography and Fourier transform ion cyclotron resonance mass spectrum, and this Fourier transform ion cyclotron resonance mass spectrum is provided with the electrospray ionization source; the full two-dimensional gas chromatography and the Fourier transform ion cyclotron resonance mass spectrum are coupled through a needle tube; the head of the needle tube is connected with the outlet of the two-dimensional chromatographic column of the full two-dimensional gas chromatograph, and the tail of the needle tube is directly arranged on an electrospray ionization source of the Fourier transform ion cyclotron resonance mass spectrum; and the needle tube is placed in an oven with the temperature of 280-300 ℃. The utility model discloses carry out the coupling with full two-dimensional gas chromatography and Fourier transform ion cyclotron resonance mass spectrum, obtained coupled system can provide super high resolution and ultra high accuracy simultaneously to can separate the isomer that boiling point and polarity are different, the specially adapted constitutes and the analysis of the geological sample of complicacy thereof.
Description
Technical Field
The utility model relates to a full two-dimentional gas chromatography and Fourier transform ion cyclotron resonance mass spectrum coupled system belongs to complicated geological sample analysis technical field.
Background
Organic mass spectrometry has been widely used for analysis of geologically complex samples (complex geological samples) including petroleum. Mass spectrometry analysis includes analysis using gas chromatography-mass spectrometry (GC-MS), two-dimensional gas chromatography-mass spectrometry (GC x GC-MS), and liquid chromatography (LC-MS). High-resolution mass spectrometry, such as time of flight mass spectrometry (TOF MS) and Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS), which have been emerging in recent years, can provide very high resolution, which can be collectively referred to as high-resolution mass spectrometry, and play an important role in the analysis of geologically complex samples. High resolution mass spectrometry is well suited for the analysis of complex mixtures because of the multiple peaks of the same mass that can be identified by it, and the mass analysis pair error is small, with FT-ICR MS mass spectrometry being well applied in the field of "petromics". However, FT-ICR MS also has some disadvantages such as that isomers having the same element cannot be identified, and that the isomers can be separated according to their boiling points by chromatography.
Therefore, providing a coupling system of a full two-dimensional gas chromatograph and a fourier transform ion cyclotron resonance mass spectrum, and using the coupling system for analyzing complex geological samples has become a technical problem to be solved in the field.
SUMMERY OF THE UTILITY MODEL
In order to solve the above disadvantages and shortcomings, the present invention provides a coupling system of full two-dimensional gas chromatography and fourier transform ion cyclotron resonance mass spectrometry.
In order to achieve the above object, the present invention provides a full two-dimensional gas chromatography and fourier transform ion cyclotron resonance mass spectrometry coupled system, wherein the coupled system comprises a full two-dimensional gas chromatography and a fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS), and the fourier transform ion cyclotron resonance mass spectrometry is provided with an electrospray ionization (ESI) source;
the full two-dimensional gas chromatography and the Fourier transform ion cyclotron resonance mass spectrum are coupled through a needle tube; the head of the needle tube is connected with the outlet of the two-dimensional chromatographic column of the full two-dimensional gas chromatograph, and the tail of the needle tube is directly arranged on an electrospray ionization source of the Fourier transform ion cyclotron resonance mass spectrum;
and the needle tube is placed in an oven with the temperature of 280-300 ℃.
According to the specific embodiment of the present invention, in the coupled system, the fourier transform ion cyclotron resonance mass spectrum provided with the electrospray ionization source can be called electrospray ionization fourier transform ion cyclotron resonance mass spectrum.
According to a specific embodiment of the present invention, the coupling system, preferably, the needle tube is made of metal.
According to an embodiment of the present invention, the coupling system, wherein, more preferably, the needle tube is a stainless steel needle tube.
According to an embodiment of the invention, in the coupling system, the needle cannula preferably has dimensions of 0.2-0.4m × 0.1mm × 0.1 μm, length × outer diameter × inner diameter.
According to an embodiment of the invention, in the coupling system, it is further preferred that the needle cannula has dimensions of 0.3m × 0.1mm × 0.1 μm, length × outer diameter × inner diameter.
According to an embodiment of the present invention, in the coupling system, preferably, the needle tube is placed in an oven maintained at 290 ℃.
According to an embodiment of the present invention, in the coupled system, preferably, the two-dimensional gas chromatography is a 7890A gas chromatography device of agilent company, usa.
According to a specific embodiment of the present invention, in the coupled system, more preferably, the one-dimensional column of the model 7890A gas chromatography device of agilent company, usa is a DB-petro type column having dimensions of 50m × 0.2mm × 0.5 μm, length × outer diameter × inner diameter;
in a specific embodiment of the invention, the temperature program of the DB-petro type column is arranged to: maintaining at 35 deg.C for 0.2min, increasing to 210 deg.C at a rate of 1.5 deg.C/min, maintaining for 0.2min, increasing to 300 deg.C at a rate of 2 deg.C/min, and maintaining for 20 min;
the two-dimensional chromatographic column of the 7890A-type gas chromatography device is a DB-17 ht-type chromatographic column, the size of which is 3m multiplied by 0.1mm multiplied by 0.1 mu m, the length multiplied by the outer diameter multiplied by the inner diameter;
in one embodiment of the present invention, the temperature ramp program for the DB-17ht type column is configured to: the temperature was maintained at 40 ℃ for 0.2min, increased to 215 ℃ at a rate of 1.5 ℃/min, maintained for 0.2min, and further increased to 305 ℃ at a rate of 2 ℃/min and maintained for 20 min.
According to an embodiment of the present invention, in the coupled system, preferably, the fourier transform ion cyclotron resonance mass spectrum is a germany BRUKER Apex-Ultra type electrospray ionization fourier transform ion cyclotron resonance mass spectrum.
In a specific embodiment of the present invention, the test condition of the fourier transform ion cyclotron resonance mass spectrum is:
the polarization voltage is +3800V, the capillary inlet voltage is +4300V, the capillary outlet voltage is-320V, the ion source six-stage rod accumulation time is 0.001s, the ion source six-stage rod direct-current voltage is 2.0V, and the radio-frequency voltage is 350 Vp-p;
the transmission optimized mass m/z of the four-stage rod Q1 is 200, and the radio frequency voltage is 400 Vp-p;
the argon flow of the collision pool is 0.30L/s, the collision energy is +1.5V, and the cumulative time of the collision pool is 1.0 s;
the flight time from the six-stage rod to the analysis cell is 10 ms;
the excitation attenuation in the analysis cell is 15dB, the trapping voltage is-6V, and the trapping deflection voltage is-3V;
the collection mass range is 150-800Da, the collection point is 2M, and the scanning spectrograms are overlapped for 64 times so as to improve the peak intensity and the signal-to-noise ratio.
According to an embodiment of the present invention, in the coupled system, preferably, the two-dimensional gas chromatography is a 7890A gas chromatography device of agilent company, usa;
the one-dimensional chromatographic column of the 7890A type gas chromatography device of Agilent, USA is a DB-petro type chromatographic column, the size of which is 50m multiplied by 0.2mm multiplied by 0.5 mu m, the length multiplied by the external diameter multiplied by the internal diameter;
the two-dimensional chromatographic column of the 7890A-type gas chromatography device is a DB-17 ht-type chromatographic column, the size of which is 3m multiplied by 0.1mm multiplied by 0.1 mu m, the length multiplied by the outer diameter multiplied by the inner diameter;
the Fourier transform ion cyclotron resonance mass spectrum is a German BRUKER Apex-Ultra type electrospray ionization Fourier transform ion cyclotron resonance mass spectrum.
The utility model discloses carry out the coupling with full two-dimensional gas chromatography and Fourier transform ion cyclotron resonance mass spectrum, obtained coupled system can provide super high resolution and ultra high accuracy simultaneously to can separate the isomer that boiling point and polarity are different, the specially adapted constitutes and the analysis of the geological sample of complicacy thereof.
Drawings
Fig. 1 is a schematic structural diagram of a full two-dimensional gas chromatography and fourier transform ion cyclotron resonance mass spectrometry coupling system provided in embodiment 1 of the present invention;
FIG. 2a is a molecular composition information map of a basic compound containing 1 nitrogen atom detected in example 2 of the present invention, wherein the one-dimensional time is 0 to 2 minutes;
FIG. 2b is a graph of molecular composition information of a basic compound containing 1 nitrogen atom detected in example 2 of the present invention, wherein the one-dimensional time is 2-4 minutes;
FIG. 2c is a graph of molecular composition information for the basic compound containing 1 nitrogen atom detected in example 2 of the present invention, wherein the one-dimensional time is 4-6 minutes;
FIG. 2d is a graph of molecular composition information for the basic compound containing 1 nitrogen atom detected in example 2 of the present invention, wherein the one-dimensional time is 6-8 minutes;
FIG. 2e is a graph of molecular composition information for the basic compound containing 1 nitrogen atom detected in example 2 of the present invention, wherein the one-dimensional time is 8-10 minutes;
FIG. 3a is a graph of molecular composition information of a basic compound containing 1 nitrogen atom detected in example 3 of the present invention, wherein the one-dimensional time is 0 to 2 minutes;
FIG. 3b is a graph of molecular composition information for a basic compound containing 1 nitrogen atom detected in example 3 of the present invention, wherein the one-dimensional time is 2-4 minutes;
FIG. 3c is a graph of molecular composition information for a basic compound containing 1 nitrogen atom detected in example 3 of the present invention, wherein the one-dimensional time is 4-6 minutes;
FIG. 3d is a graph of molecular composition information for the basic compound containing 1 nitrogen atom detected in example 3 of the present invention, wherein the one-dimensional time is 6-8 minutes;
FIG. 3e is a graph of molecular composition information for the basic compound containing 1 nitrogen atom detected in example 3 of the present invention, wherein the one-dimensional time is 8-10 minutes;
FIG. 4 is a molecular composition information map of a basic compound containing 1 nitrogen atom detected in comparative example 1 of the present invention;
fig. 5 is a molecular composition information map of a basic compound containing 1 nitrogen atom detected in comparative example 2 of the present invention.
The main reference numbers illustrate:
1. a two-dimensional chromatographic column;
2. a chromatographic column oven;
3. pressing the cap;
4. a stainless steel needle tube;
5. a needle tube oven;
6. an electrospray ionization source.
Detailed Description
The following detailed description of the embodiments and the advantageous effects thereof will be provided by way of specific examples and accompanying drawings, which are provided to assist the reader in better understanding the nature and features of the present invention, and are not intended to limit the scope of the present invention.
Example 1
The embodiment provides a full two-dimensional gas chromatography and fourier transform ion cyclotron resonance mass spectrometry coupled system, a structural schematic diagram of which is shown in fig. 1, and as can be seen from fig. 1, the system includes:
the system comprises a full two-dimensional gas chromatograph and a Fourier transform ion cyclotron resonance mass spectrum, wherein the Fourier transform ion cyclotron resonance mass spectrum is provided with an electrospray ionization source;
the full two-dimensional gas chromatography and the Fourier transform ion cyclotron resonance mass spectrum are coupled through a stainless steel needle tube 4; the head of the stainless steel needle tube is connected with the outlet of the two-dimensional chromatographic column 1 of the full two-dimensional gas chromatograph through a pressing cap 3, and the tail of the stainless steel needle tube is directly arranged on an electrospray ionization source 6 of the Fourier transform ion cyclotron resonance mass spectrum;
and the stainless steel needle tube is placed in a needle tube oven 5 with the temperature kept at 290 ℃.
In this embodiment, the two-dimensional chromatographic column 1 is located in a chromatographic column oven 2.
In this embodiment, the stainless steel needle tube has dimensions of 0.3m × 0.1mm × 0.1 μm, length × outer diameter × inner diameter.
In this embodiment, the full-two-dimensional gas chromatography is a 7890A gas chromatography apparatus of agilent corporation, usa;
the one-dimensional chromatographic column of the 7890A type gas chromatography device of Agilent, USA is a DB-petro type chromatographic column, the size of which is 50m multiplied by 0.2mm multiplied by 0.5 mu m, the length multiplied by the external diameter multiplied by the internal diameter;
the two-dimensional column of the 7890A type gas chromatography device was a DB-17ht type column, and had dimensions of 3 m.times.0.1 mm.times.0.1. mu.m, length. times.outer diameter. times.inner diameter.
The Fourier transform ion cyclotron resonance mass spectrum is a German BRUKER Apex-Ultra type electrospray ionization Fourier transform ion cyclotron resonance mass spectrum.
Example 2
The embodiment provides a method for analyzing petroleum components by coupling full-two-dimensional gas chromatography and electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry, wherein the method utilizes the coupling system provided by the embodiment 1, and comprises the following steps:
coupling 7890A type gas chromatography of Agilent company and BRUKER Apex-Ultra type electro-spray ionization Fourier transform ion cyclotron resonance mass spectrometry of Germany to obtain a coupled system;
wherein the 7890A type gas chromatography equipped one-dimensional column is a DB-petro type column (dimensions 50 m.times.0.2 mm.times.0.5 μm, length. times.OD. times.ID.), and the temperature rise program is set as follows: maintaining at 35 deg.C for 0.2min, increasing to 210 deg.C at a rate of 1.5 deg.C/min, maintaining for 0.2min, and increasing to 300 deg.C at a rate of 2 deg.C/min and maintaining for 20 min;
7890 type A gas chromatography was equipped with a DB-17ht type column (dimensions 3 m.times.0.1 mm.times.0.1 μm, length. times.outer diameter. times.inner diameter), and the temperature program was set to: maintaining at 40 deg.C for 0.2min, increasing to 215 deg.C at 1.5 deg.C/min, maintaining for 0.2min, increasing to 305 deg.C at 2 deg.C/min, and maintaining for 20 min;
the interface between 7890 type A gas chromatography and BRUKER Apex-Ultra type electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry, Germany, is a stainless steel needle tube (with dimensions of 0.3m x 0.1mm x 0.1 μm, length x outer diameter x inner diameter) placed in a needle tube oven with a temperature of 290 ℃. The head of the needle tube is connected with the outlet of a two-dimensional chromatographic column of 7890A-type gas chromatography, and the tail of the needle tube is directly arranged on an electrospray ionization source of German BRUKER Apex-Ultra type electrospray ionization Fourier transform ion cyclotron resonance mass spectrum;
the method for analyzing the petroleum components is specifically carried out according to the following steps:
dissolving 2 mu L of petroleum sample A in 1mL of dichloromethane, injecting 7890A type gas chromatography, taking helium as carrier gas, ionizing the sample in an ESI source of electrospray ionization Fourier transform ion cyclotron resonance mass spectrum after the sample passes through a one-dimensional chromatographic column and a two-dimensional chromatographic column of the 7890A type gas chromatography in an electrospray mode, and then analyzing the sample in Fourier transform ion cyclotron resonance mass spectrum;
the test conditions of the FT-ICR MS system are as follows:
the polarization voltage is +3800V, the capillary inlet voltage is +4300V, the capillary outlet voltage is-320V, the ion source six-stage rod accumulation time is 0.001s, the ion source six-stage rod direct-current voltage is 2.0V, and the radio-frequency voltage is 350 Vp-p; the transmission optimized mass m/z of the four-stage rod Q1 is 200, and the radio frequency voltage is 400 Vp-p; the argon flow of the collision pool is 0.30L/s, the collision energy is +1.5V, and the cumulative time of the collision pool is 1.0 s; the flight time from the six-stage rod to the analysis cell is 10 ms; the excitation attenuation in the analysis cell is 15dB, the trapping voltage is-6V, and the trapping deflection voltage is-3V; the collection mass range is 150-800Da, the collection point is 2M, and the scanning spectrograms are overlapped for 64 times so as to improve the peak intensity and the signal-to-noise ratio.
Molecular composition information maps of the basic compound containing 1 nitrogen atom (referred to as N1 compound for short) detected in the example are shown in FIGS. 2 a-2 e, and as can be seen from FIGS. 2 a-2 e, N1 compound is detected in the example 2 at one-dimensional time of 0-2 min, 2-4 min, 4-6 min, 6-8 min and 8-10 min, wherein the carbon number distribution range of the N1 compound detected at 0-2 min is 3-15, and the equivalent double bond number is 0-2; the carbon number distribution range of the N1 compounds detected in 2-4 minutes is 4-19, and the equivalent double bond number is 0-2; the carbon number distribution range of the N1 compounds detected in 4-6 minutes is 4-16, and the equivalent double bond number is 0-4; the carbon number distribution range of the N1 compounds detected in 6-8 minutes is 6-15, and the equivalent double bond number is 0-1; the carbon number distribution range of the N1 compounds detected in 8-10 minutes is 5-25, and the equivalent double bond number is 0-4.
Example 3
The embodiment provides a method for analyzing petroleum components by coupling full-two-dimensional gas chromatography and electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry, wherein the method utilizes the coupling system provided by the embodiment 1, and comprises the following steps:
coupling 7890A type gas chromatography of Agilent company and BRUKER Apex-Ultra type electro-spray ionization Fourier transform ion cyclotron resonance mass spectrometry of Germany to obtain a coupled system;
among them, the 7890A type gas chromatography-equipped one-dimensional column was a DB-petro type column (the dimensions of which were 50 m.times.0.2 mm.times.0.5. mu.m, length. times.outer diameter. times.inner diameter), and the temperature-raising program was set as follows: maintaining at 35 deg.C for 0.2min, increasing to 210 deg.C at a rate of 1.5 deg.C/min, maintaining for 0.2min, and increasing to 300 deg.C at a rate of 2 deg.C/min and maintaining for 20 min; 7890 type A gas chromatography was equipped with a DB-17ht type column (dimensions 3 m.times.0.1 mm.times.0.1 μm, length. times.outer diameter. times.inner diameter), and the temperature program was set to: maintaining at 40 deg.C for 0.2min, increasing to 215 deg.C at 1.5 deg.C/min, maintaining for 0.2min, increasing to 305 deg.C at 2 deg.C/min, and maintaining for 20 min;
the interface between 7890 type A gas chromatography and BRUKER Apex-Ultra type electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry, Germany, is a stainless steel needle tube (with dimensions of 0.3m x 0.1mm x 0.1 μm, length x outer diameter x inner diameter) placed in a needle tube oven with a temperature of 290 ℃. The needle tube head is connected with the outlet of a 7890A type gas chromatography two-dimensional chromatographic column, and the tail part is directly arranged on an ESI source of German BRUKER Apex-Ultra type electrospray ionization Fourier transform ion cyclotron resonance mass spectrum.
The method for analyzing the petroleum components is specifically carried out according to the following steps:
dissolving a 2 mu L petroleum sample B in 1mL dichloromethane, injecting into a two-dimensional gas chromatograph, taking helium as carrier gas, passing the sample through a one-dimensional chromatographic column and a two-dimensional chromatographic column of a 7890A type gas chromatograph, ionizing in an ESI source of the electrospray ionization Fourier transform ion cyclotron resonance mass spectrum in an electrospray mode, and then entering into a Fourier transform ion cyclotron resonance mass spectrum for analysis;
the test conditions of the FT-ICR MS system are as follows:
the polarization voltage is +3800V, the capillary inlet voltage is +4300V, the capillary outlet voltage is-320V, the ion source six-stage rod accumulation time is 0.001s, the ion source six-stage rod direct-current voltage is 2.0V, and the radio-frequency voltage is 350 Vp-p; the transmission optimized mass m/z of the four-stage rod Q1 is 200, and the radio frequency voltage is 400 Vp-p; the argon flow of the collision pool is 0.30L/s, the collision energy is +1.5V, and the cumulative time of the collision pool is 1.0 s; the flight time from the six-stage rod to the analysis cell is 10 ms; the excitation attenuation in the analysis cell is 15dB, the trapping voltage is-6V, and the trapping deflection voltage is-3V; the collection mass range is 150-800Da, the collection point is 2M, and the scanning spectrograms are overlapped for 64 times so as to improve the peak intensity and the signal-to-noise ratio.
Molecular composition information maps of the basic compound containing 1 nitrogen atom (abbreviated as N1 compound) detected in this example are shown in fig. 3 a-3 e, and as can be seen from fig. 3 a-3 e, N1 compound is detected in example 3 at one-dimensional time of 0-2 min, 2-4 min, 4-6 min, 6-8 min and 8-10 min, wherein the carbon number distribution range of N1 compound detected at 0-2 min is 3-20, and the equivalent double bond number is 0-5; the carbon number distribution range of the N1 compounds detected in 2-4 minutes is 4-16, and the equivalent double bond number is 0-1; the carbon number distribution range of the N1 compounds detected in 4-6 minutes is 3-22, and the equivalent double bond number is 0-4; the carbon number distribution range of the N1 compounds detected in 6-8 minutes is 2-21, and the equivalent double bond number is 0-3; the carbon number distribution range of the N1 compounds detected in 8-10 minutes is 2-26, and the equivalent double bond number is 0-2.
Comparative example 1
The present comparative example provides a method of analyzing a petroleum component directly using electrospray ionization fourier transform ion cyclotron resonance mass spectrometry, wherein the method comprises the steps of:
dissolving 2 mu L of petroleum sample A in 1mL of dichloromethane, directly injecting into an ESI source of the electrospray ionization Fourier transform ion cyclotron resonance mass spectrum, ionizing in an electrospray mode, and then entering into a Fourier transform ion cyclotron resonance mass spectrum of the electrospray ionization Fourier transform ion cyclotron resonance mass spectrum for analysis;
the test conditions of the FT-ICR MS system are as follows:
the polarization voltage is +3800V, the capillary inlet voltage is +4300V, the capillary outlet voltage is-320V, the ion source six-stage rod accumulation time is 0.001s, the ion source six-stage rod direct-current voltage is 2.0V, and the radio-frequency voltage is 350 Vp-p; the transmission optimized mass m/z of the four-stage rod Q1 is 200, and the radio frequency voltage is 400 Vp-p; the argon flow of the collision pool is 0.30L/s, the collision energy is +1.5V, and the cumulative time of the collision pool is 1.0 s; the flight time from the six-stage rod to the analysis cell is 10 ms; the excitation attenuation in the analysis cell is 15dB, the trapping voltage is-6V, and the trapping deflection voltage is-3V; the collection mass range is 150-800Da, the collection point is 2M, and the scanning spectrograms are overlapped for 64 times so as to improve the peak intensity and the signal-to-noise ratio.
The molecular composition information spectrum of the N1-based compound detected in comparative example 1 is shown in fig. 4, and it can be seen from fig. 4 that the carbon number distribution range of the N1-based compound detected in comparative example 1 is 4 to 22, the equivalent double bond number is 0 to 1, which is significantly less than the molecular composition information of the N1-based compound detected in example 2.
Comparative example 2
The present comparative example provides a method of analyzing petroleum fractions directly using electrospray ionization fourier transform ion cyclotron resonance mass spectrometry, wherein the method comprises the steps of:
dissolving 2 mu L of petroleum sample B in 1mL of dichloromethane, directly injecting into an ESI source of the electrospray ionization Fourier transform ion cyclotron resonance mass spectrum, ionizing in an electrospray mode, and then entering into a Fourier transform ion cyclotron resonance mass spectrum of the electrospray ionization Fourier transform ion cyclotron resonance mass spectrum for analysis;
the test conditions of the FT-ICR MS system are as follows:
the polarization voltage is +3800V, the capillary inlet voltage is +4300V, the capillary outlet voltage is-320V, the ion source six-stage rod accumulation time is 0.001s, the ion source six-stage rod direct-current voltage is 2.0V, and the radio-frequency voltage is 350 Vp-p; the transmission optimized mass m/z of the four-stage rod Q1 is 200, and the radio frequency voltage is 400 Vp-p; the argon flow of the collision pool is 0.30L/s, the collision energy is +1.5V, and the cumulative time of the collision pool is 1.0 s; the flight time from the six-stage rod to the analysis cell is 10 ms; the excitation attenuation in the analysis cell is 15dB, the trapping voltage is-6V, and the trapping deflection voltage is-3V; the collection mass range is 150-800Da, the collection point is 2M, and the scanning spectrograms are overlapped for 64 times so as to improve the peak intensity and the signal-to-noise ratio.
The molecular composition information spectrum of the N1-based compound detected in comparative example 2 is shown in fig. 5, and it can be seen from fig. 5 that the N1-based compound detected in comparative example 2 has a carbon number distribution ranging from 3 to 24 and an equivalent double bond number ranging from 0 to 1, which is significantly less than the molecular composition information of the N1-based compound detected in example 3.
Therefore, the embodiment of the utility model provides a this coupled system is the device of a full two-dimensional gas chromatography and the coupling of electrospray ionization Fourier transform ion cyclotron resonance mass spectrum, the utility model discloses this coupled system combines full two-dimensional gas chromatography to the high-efficient separation of complex mixture and the super high resolution ratio and the accuracy nature of electrospray ionization Fourier transform ion cyclotron resonance mass spectrum, and this coupled system can be used to the characterization of complex systems such as hydrocarbon source rock organic matter and oil, still can obtain the accurate quality of retention time and every compound simultaneously.
The above description is only for the specific embodiments of the present invention, and the scope of the present invention can not be limited by the embodiments, so that the replacement of the equivalent components or the equivalent changes and modifications made according to the protection scope of the present invention should still belong to the scope covered by the present patent.
Claims (12)
1. A full two-dimensional gas chromatography and Fourier transform ion cyclotron resonance mass spectrum coupling system is characterized in that the coupling system comprises a full two-dimensional gas chromatography and a Fourier transform ion cyclotron resonance mass spectrum, and the Fourier transform ion cyclotron resonance mass spectrum is provided with an electrospray ionization source;
the full two-dimensional gas chromatography and the Fourier transform ion cyclotron resonance mass spectrum are coupled through a needle tube; the head of the needle tube is connected with the outlet of the two-dimensional chromatographic column of the full two-dimensional gas chromatograph, and the tail of the needle tube is directly arranged on an electrospray ionization source of the Fourier transform ion cyclotron resonance mass spectrum;
and the needle tube is placed in an oven with the temperature of 280-300 ℃.
2. The coupling system of claim 1, wherein the needle cannula is a metallic needle cannula.
3. The coupling system of claim 2, wherein the needle cannula is a stainless steel needle cannula.
4. The coupling system of any one of claims 1-3, wherein the needle cannula has dimensions of 0.2-0.4m x 0.1mm x 0.1 μm, length x outer diameter x inner diameter.
5. The coupling system of claim 4, wherein the needle cannula has dimensions of 0.3m x 0.1mm x 0.1 μm, length x outer diameter x inner diameter.
6. The coupling system of any one of claims 1-3, wherein the needle cannula is placed in an oven maintained at a temperature of 290 ℃.
7. The coupling system of claim 4, wherein the syringe is placed in an oven maintained at a temperature of 290 ℃.
8. The coupling system of claim 5, wherein the syringe is placed in an oven maintained at a temperature of 290 ℃.
9. The coupling system of any one of claims 1-3, wherein the full two-dimensional gas chromatograph is a model 7890A gas chromatograph unit from Agilent, USA.
10. The coupling system of claim 9, wherein the one-dimensional chromatography column of the agilent 7890A gas chromatography device is a DB-petro type chromatography column having dimensions 50m x 0.2mm x 0.5 μm, length x outer diameter x inner diameter;
the two-dimensional column of the 7890A type gas chromatography device was a DB-17ht type column, and had dimensions of 3 m.times.0.1 mm.times.0.1. mu.m, length. times.outer diameter. times.inner diameter.
11. The coupled system of any of claims 1-3, wherein the Fourier transform ion cyclotron resonance mass spectrum is an electrospray ionization Fourier transform ion cyclotron resonance mass spectrum of the Germany BRUKER Apex-Ultra type.
12. The coupling system of any one of claims 1-3, wherein the full two-dimensional gas chromatograph is a model 7890A gas chromatograph unit from Agilent, USA;
the one-dimensional chromatographic column of the 7890A type gas chromatography device of Agilent, USA is a DB-petro type chromatographic column, the size of which is 50m multiplied by 0.2mm multiplied by 0.5 mu m, the length multiplied by the external diameter multiplied by the internal diameter;
the two-dimensional chromatographic column of the 7890A-type gas chromatography device is a DB-17 ht-type chromatographic column, the size of which is 3m multiplied by 0.1mm multiplied by 0.1 mu m, the length multiplied by the outer diameter multiplied by the inner diameter;
the Fourier transform ion cyclotron resonance mass spectrum is a German BRUKER Apex-Ultra type electrospray ionization Fourier transform ion cyclotron resonance mass spectrum.
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| WO2021212920A1 (en) * | 2020-12-08 | 2021-10-28 | 广东省科学院测试分析研究所(中国广州分析测试中心) | Nanoliter spray-fticr-ms analysis method and device for organic matter dissolved in environmental solid sample |
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