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Method and apparatus for isotope ratio mass spectrometry

An isotope ratio mass spectrometry and isotope ratio technology, applied in the field of mass spectrometry, can solve problems such as the accuracy and accuracy of isotope ratio measurement, system complexity, etc.

Active Publication Date: 2018-08-14
THERMO FISHER SCI BREMEN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the step of removing the sample from the main stream into the loop and then filling the mass spectrometer has not achieved the level of precision and accuracy typically required for isotope ratio measurements
In addition, the system is complex and requires an additional sample loop and a second pump system

Method used

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  • Method and apparatus for isotope ratio mass spectrometry
  • Method and apparatus for isotope ratio mass spectrometry
  • Method and apparatus for isotope ratio mass spectrometry

Examples

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Effect test

example 1

[0124] Example 1 - Injection Measurement (Comparative Example)

[0125] Sample solutions of the samples listed in Table 1 in methanol / water 50:50 (v:v) were prepared at approximately 10 μg / ml and injected directly into standard Thermo Scientific in an orbitrap mass spectrometer. A schematic diagram of the instrument is shown in Figure 4 In, the instrument is a preferred mass spectrometer for use in the present invention. The mass spectrometer 200 includes an electrospray ion source 202 that generates ions that enter an RF lens 204 before being directed by active beam-steering ion optics 206 to a quadrupole mass filter 208 . The mass isolation window can be set by the mass filter to emit ions of a desired mass to the downstream ion trap (C-trap) 210, where the ions can accumulate before ejecting the ions to the orbitrap mass analyzer 212 for mass analysis. If desired, the ions can be emitted through the C-trap 210 to a downstream higher energy collisional dissociation (H...

example 2

[0138] Example 2 - LC / MS measurement without reduced flow (comparative example)

[0139] Solutions of the samples listed in Table 1 in methanol / water 20:80 at 10 μg / ml (+ / −0.02 μg / ml) were used in the experiments. Such as figure 2 The LC / MS system schematically shown in was used with the following LC setup:

[0140] - Thermo Fisher Scientific with autosampler and quaternary pump system

[0141] - 10 μl injection (corresponding to 100ng injection)

[0142] -Thermo Fisher Scientific Accucore aQ column; 2.1×100mm, 2.6mm particle size

[0143] - Solvent A: water, 0.1% formic acid (FA), 2 mM ammonium acetate

[0144] - Solvent B: methanol, 0.1% FA, 2 mM ammonium acetate

[0145] - Solvent Gradient 100% A (0 to 0.5 minutes); 50% A / 50% B (0.5 to 3.0 minutes); 20% A / 80% B (3.0 to 3.3 minutes); 100% A (3.3 to 5 minutes) . Figure 8 The solvent step gradient used in the experiment is shown.

[0146] Operate the mass spectrometer with the following parameters:

[0147] - Ma...

example 3

[0161] Example 3: LC / MS measurements with reduced flow

[0162] Sample solutions of the samples listed in Table 1 in methanol / water 20:80 at 10 μg / ml (+ / −0.02 μg / ml) were used in the experiments. Such as image 3 The LC / MS system schematically shown in was used with the following LC setup:

[0163] - Thermo Fisher Scientific with autosampler and quaternary pump

[0164] - 10 μl injection (corresponding to 100ng injection)

[0165] -Thermo Fisher Scientific Accucore aQ column; 2.1100mm×, 2.6mm particle size

[0166] - Solvent A: water, 0.1% FA, 2mM ammonium acetate

[0167] - Solvent B: methanol, 0.1% FA, 2 mM ammonium acetate

[0168] - Gradient 100% A (0 to 0.5 minutes); 50% A / 50% B (0.5 to 8.5 minutes); 20% A / 80% B (8.5 to 9.0 minutes); 100% A (9.0 to 11.0 minutes) ( step gradient)

[0169] - Diverter valve switched at t=2.75 min and t=8.00 min

[0170] Figure 11 The solvent step gradient used in the experiment is shown. In this experiment, a reduced flow sett...

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Abstract

The application relates to a method and apparatus for isotope ratio mass spectrometry. The method of isotope ratio mass spectrometry comprises: flowing a liquid mobile phase that contains a sample through a separation device, the sample comprising at least one molecular species having an isotope ratio to be determined; setting or reducing the flow rate of the liquid mobile phase flowing through the separation device for at least a portion of time that the at least one molecular species is emerging from the separation device to achieve a desired isotope ratio precision; mass analyzing the at least one molecular species that has emerged from the separation device at least while the flow rate is set or reduced; and determining from the mass analysis at least one isotope ratio of the at leastone molecular species from the intensities of mass peaks of at least two isotopologues of the at least one molecular species, wherein the mass analysis is performed with mass resolving power high enough to resolve the two most abundant mass peaks at the nominal mass of at least one of the isotopologues.

Description

technical field [0001] The present invention relates to the field of mass spectrometry. In particular, the present invention relates to isotope ratio mass spectrometry (IRMS), and more particularly to IRMS coupled to liquid chromatography. The present invention provides both methods and apparatus. Background technique [0002] Accurate and precise isotope measurements are routinely performed on magnetic sector mass spectrometers, particularly those utilizing multiple collectors for simultaneous detection of isotopes. Prior to analysis, samples are typically subjected to oxidation, pyrolysis, and / or reduction at elevated temperatures to produce gaseous molecules such as CO x , NO x , N 2 、H 2 O and SO 2 One or more of (x=1 or 2). The gas is then introduced into an isotope ratio mass spectrometer for isotope analysis. In an isotope ratio mass spectrometer, a gas is ionized and the ratio of the corresponding isotopes is measured, for example by comparing the outputs of ...

Claims

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Application Information

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IPC IPC(8): G01N27/62
CPCG01N27/62G01N30/8658G01N2030/324H01J49/0031G01N30/7233H01J49/0036H01J49/38H01J49/40H01J49/282H01J49/0459
Inventor J·格力普-拉敏
Owner THERMO FISHER SCI BREMEN
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