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Method for applying acetophenone derivatives to unsaturated lipid analysis

An analytical method, an unsaturated technique, applied in the field of mass spectrometry, which can solve the problem that lipidomics is not widely used

Active Publication Date: 2020-08-07
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, their use in lipidomics is not yet widespread, limited by instrument modification and complexity requirements

Method used

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  • Method for applying acetophenone derivatives to unsaturated lipid analysis
  • Method for applying acetophenone derivatives to unsaturated lipid analysis
  • Method for applying acetophenone derivatives to unsaturated lipid analysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1 Analysis of C=C position on the fatty acid chain of phosphatidylcholine standard PC 16:0 / 18:1 (9Z) by sodium spray method

[0044] Preparation of analytical samples: 5 μM PC 16:0 / 18:1 (9Z) was dissolved in 1:1 acetonitrile:20 mM ammonium acetate aqueous solution, and the solution also contained 2 mM triFAP.

[0045] Mass Spectrometry:

[0046] (1) The analytical sample PC 16:0 / 18:1 (9Z) was deoxygenated under nitrogen flow for about 5 minutes, and then loaded into the offline microfluidic reaction device. The reaction time is controlled at about 20s, and the reacted liquid is loaded into the sodium nozzle for mass spectrometry detection.

[0047] (2) Firstly, the unreacted solution is detected, and the stainless steel wire is inserted into the liquid of the analysis sample.

[0048] (3) In the positive ion PIS 184 mode, the lipid species was identified as phosphatidylcholine. Mass spectrometry parameters were set as follows: curtain gas 10psi; collision gas...

Embodiment 2

[0052]Mass spectrometry analysis of PC 16:0 / 18:1 was performed with reference to a method similar to that of Example 1, the difference being that FMAP was used for the acetophenone derivative. image 3 a is the primary mass spectrum after the reaction of PC 16:0 / 18:1 (5μM) and 2mM FMAP; image 3 b is the CID spectrum of the reaction product of PC 16:0 / 18:1 (collision energy is around 40eV); image 3 c is the chromatogram of the PC 16:0 / 18:1 reaction product separated by a reversed-phase chromatographic column, and the extracted ion is m / z 948.6 in the primary spectrum; image 3 d is the chromatogram of PC 16:0 / 18:1 reaction product separated by reversed-phase chromatographic column, the extracted ion is the fragment ion m / z 930.6(-H in the secondary spectrum 2 O), m / z 760.6 (-R), m / z 806.5 (F O ) and m / z 650.5 (F A ).

Embodiment 3

[0053] Example 3 Liquid Chromatography-Mass Spectrometry Analysis of the C=C Position of Lipid Molecules in Bovine Liver Lipid Extract

[0054] Preparation of analytical samples: 50 ppm bovine liver lipid extract dissolved in methanol

[0055] Mass Spectrometry:

[0056] (1) In the positive ion mode, neutral loss scans at 141Da, 185Da, 172Da and 260Da respectively obtained phosphatidylethanolamine (PE), phosphatidylserine (PS), phosphatidylglycerol (PG) and phosphatidylinositol (PI) Distribution information, the precursor ion scans m / z 184 to obtain the distribution information of PC (such as Figure 6 c). Mass spectrometry parameters were set as follows: curtain gas 30psi; collision gas high; voltage 4500V; temperature 400°C; spray gas 30psi; auxiliary heating gas 30psi; declustering voltage 80eV; collision energy 45eV. The liquid chromatography conditions are mobile phase A: 10 mM ammonium acetate aqueous solution, and mobile phase B: acetonitrile solution containing 0.2%...

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Abstract

The invention discloses a method for carrying out structural analysis on lipid double-bond positions by combining photochemical derivation and tandem mass spectrometry. Double bonds on a lipid aliphatic chain and acetophenone derivatives 2 ', 4', 6 '-trifluoroacetophenone (triFAP) or 4'-trifluoromethyl acetophenone (FMAP) are subjected to an efficient PB reaction under excitation of 254-nanometerultraviolet light, so that a pair of isomer products containing a four-membered ring structure is formed. In the tandem mass spectrometry, the pair of isomer products is capable of generating a pair of diagnostic ions having a fixed mass-to-charge ratio for the determination of a carbon-carbon double-bond position. For a lipid containing a plurality of carbon-carbon double bond position isomers atthe same time, the relative content of each isomer can be directly obtained by utilizing the intensity ratio of the diagnostic ions. The method can be combined with a shotgun method or liquid chromatography separation to realize high-flux, high-sensitivity and fine structure analysis of lipids in a complex sample.

Description

technical field [0001] The present invention relates to the technical field of mass spectrometry, in particular to a method for the application of acetophenone derivatives in the analysis of unsaturated lipids, and more specifically to the use of lipids and acetophenone derivatives in mass spectrometry High-throughput mass spectrometry detection and analysis of its fine structure. Background technique [0002] Lipids are important structural scaffolds of cell membranes and are involved in a variety of cell signaling and metabolic processes. One important subclass, unsaturated lipids, is characterized by at least one carbon-carbon double bond (C=C) on the alkyl chain distributed. Relevant studies have shown that the distribution of unsaturated lipids presents regular changes in the relevant organelles involved in the secretory pathway and in some differentiation structures such as nerve axons; and the ratio of C=C isomers has been confirmed in breast cancer cells and T2D pat...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/7233G01N30/8679
Inventor 瑕瑜赵婧
Owner TSINGHUA UNIV
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