Method for rapidly detecting compound with instable structure

A detection method and compound technology, applied in the field of analytical chemistry, can solve problems such as false positive results and low sensitivity, achieve high-throughput analysis, improve detection sensitivity, and facilitate qualitative analysis

Inactive Publication Date: 2013-01-02
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although the Dart ion source has been successfully used, it has the disadvantages of low sensitivity and the observation of fragments of some compounds, which raises the question of whether a particular ion in the mass spectrum of a mixture represents a compound or just a certain ion. Fragments of a compound may produce false positive results. So far, there has been no report on the use of Dart ion sources to analyze structurally unstable compounds. Solving this problem is very important and has very important practical significance

Method used

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  • Method for rapidly detecting compound with instable structure
  • Method for rapidly detecting compound with instable structure
  • Method for rapidly detecting compound with instable structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Prepare the glucose and methanol solution into a glucose-methanol solution with a concentration of 0.5 mg / mL;

[0036] Accurately weigh 10 μL of glucose-methanol solution and place it on the sieve, and after natural drying in the air, place the sieve on a real-time direct analysis mass spectrometry ion source (IonSense, Inc., Saugus, MA, USA) with a gas outlet and a Finnigan LTQ TM Between the ion inlets of a linear ion trap mass spectrometer (San Jose, CA, USA), the real-time direct analysis mass spectrometry ion source conditions are as follows: negative ion mode, discharge needle voltage 3kV, grid voltage 250V, working gas is high-purity argon, gas temperature 300°C, gas pressure 0.4MPa; linear ion trap mass spectrometer conditions are as follows: negative ion mode, capillary voltage -20V, lens voltage -70V, capillary temperature 250°C, scan range mass-to-charge ratio (m / z) 140~200Da.

[0037] figure 1 The ion of m / z179.1 represents the molecular ion peak of glucose...

Embodiment 2

[0040] Prepare 2'-deoxycytidine and methanol solution into a 2'-deoxycytidine-methanol solution with a concentration of 0.5 mg / mL;

[0041] Accurately weigh 10 μL of 2'-deoxycytidine-methanol solution and place it on the sieve, and after drying naturally in the air, place the sieve in a real-time direct analysis mass spectrometry ion source (IonSense, Inc., Saugus, MA, USA) with the gas outlet and Finnigan LTQ TM Between the ion inlets of a linear ion trap mass spectrometer (San Jose, CA, USA), the real-time direct analysis mass spectrometry ion source conditions are as follows: positive ion mode, discharge needle voltage 3kV, grid voltage 350V, working gas is high-purity argon, gas The temperature is 300°C, the gas pressure is 0.4MPa; the conditions of the linear ion trap mass spectrometer are as follows: positive ion mode, capillary voltage 25V, lens voltage 80V, capillary temperature 250°C, scan range mass-to-charge ratio (m / z) 80~700Da.

[0042] image 3 Medium m / z81.2, ...

Embodiment 3

[0046] Prepare 2,4,6-trihydroxyacetophenone and methanol solution into a 2'-deoxycytidine-methanol solution with a concentration of 2.5mM;

[0047] Accurately weigh 10 μL of 2'-deoxycytidine-methanol solution and place it on the sieve. After drying naturally in the air, place the sieve in a real-time direct analysis mass spectrometry ion source (IonSense, Inc., Saugus, MA, USA) with the gas outlet and Finnigan LTQ TM Between the ion inlets of a linear ion trap mass spectrometer (San Jose, CA, USA), the real-time direct analysis mass spectrometer ion source conditions are as follows: positive ion mode, discharge needle voltage 3kV, grid voltage 350V, working gas is high-purity argon, gas The temperature is 300°C, the gas pressure is 0.4MPa; the instrument conditions of the linear ion trap mass spectrometer are as follows: positive ion mode, capillary voltage 20V, lens voltage 75V, capillary temperature 250°C, scan range mass-to-charge ratio (m / z) 130~190Da.

[0048] Figure 5...

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Abstract

The invention discloses a method for rapidly detecting a compound with an instable structure and belongs to the technical field of analysis chemistry, solving the problem that the existing method can not accurately and rapidly detect the compound with the instable structure. The method comprises the following steps of: accurately weighing 10 mu L of compound with the instable structure on a screen, naturally drying the compound in the air; and placing the compound between a real-time direct analysis mass spectrometer ion source gas outlet and a linear ion trap mass spectrometer ion inlet, wherein when the ion source is in a positive or negative ion mode, the spray point voltage is 3kV, the grid voltage is 250 to 500V, the working gas is high-purity argon, the temperature is 200 to 500 DEG C and the pressure is 0.3 to 0.8MPa, and when the mass spectrometer is in a positive or negative ion mode, the capillary voltage is respectively 10 to 50V and 10 to 50V below zero, the lens voltage is respectively 50 to 150V and 50 to 150V below zero, the capillary temperature is 250 to 300 DEGC, and the mass-to-charge ratio in a scanning range is 60 to 700Da. The method is accurate, quick and high in sensitivity.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a rapid detection method for structurally unstable compounds. Background technique [0002] In 2003, Cody et al. invented the real-time direct analysis mass spectrometry ion source, that is, the Dart ion source, which can quickly analyze solid, liquid and gaseous substances under open atmospheric conditions, without the need to process samples, and Dart does not produce adducted ions (such as adding sodium or Molecular ions of potassium), positive charges only have protonated ions, negative charges only have deprotonated ions, the mass spectrum is more concise, qualitative analysis is easier to achieve, Dart mass spectrometry has high throughput, relatively low ion suppression, lack of memory effect, It is widely used in reaction monitoring, forensic science, detection of counterfeit and inferior drugs, fruit and food analysis and metabolomics research, etc. The pri...

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N27/626
Inventor 杨洪梅刘淑莹万德彬连文慧陈宁
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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