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CN-121994572-A - Lanthanide metal-1, 3-diketone complex detection method based on MALDI-TOF MS

CN121994572ACN 121994572 ACN121994572 ACN 121994572ACN-121994572-A

Abstract

The application discloses a detection method of lanthanide metal-1, 3-diketone complex based on MALDI-TOF MS, which comprises the following steps of preparing a detection sample of the lanthanide metal-1, 3-diketone complex, adopting a reflection mode for detection, adopting a laser intensity of 45-55% and a voltage multiple of 13.9X, and adopting MALDI-TOF MS for detection after sample application under the room temperature condition to obtain a relative molecular mass and isotope distribution result. The method provided by the application can be used for detecting the lanthanide metal-1, 3-diketone complex by MALDI-TOF MS to obtain the molecular ion peak of the lanthanide metal-1, 3-diketone complex molecule, the error of the detection result is less than 5ppm, and the detection requirement of high-resolution mass spectrum is met.

Inventors

  • DAI GUOXIN
  • YE YE

Assignees

  • 中国科学院昆明植物研究所

Dates

Publication Date
20260508
Application Date
20260326

Claims (9)

  1. 1. The lanthanide metal-1, 3-diketone complex detection method based on MALDI-TOF MS is characterized by comprising the following steps: after a detection sample of the lanthanide metal-1, 3-diketone complex is prepared, reflection mode detection is adopted, the laser intensity is 45-55%, the voltage multiple is 13.9×, and detection is carried out by MALDI-TOF MS after sample application under the room temperature condition to obtain the relative molecular mass and isotope distribution result.
  2. 2. The method for detecting lanthanide metal-1, 3-dione complex based on MALDI-TOF MS according to claim 1, wherein the preparation of the detection sample comprises the steps of: dissolving lanthanide metal-1, 3-diketone complex to obtain lanthanide metal-1, 3-diketone complex solution; uniformly mixing lanthanide metal-1, 3-diketone complex solution and DHB matrix solution to obtain a detection sample; The concentration of the lanthanide metal-1, 3-dione complex solution in the test sample was 1 mg/mL.
  3. 3. The method for detecting lanthanide metal-1, 3-dione complex based on MALDI-TOF MS according to claim 2, wherein the preparation of DHB matrix solution comprises the steps of: the solution was dissolved in TA30 as a solvent, and a sodium chloride solution having a concentration of 0.5 mM and a potassium chloride solution having a concentration of 0.5 mM were added to prepare a DHB base solution having a concentration of 20 mg/mL.
  4. 4. The method for detecting lanthanide metal-1, 3-dione complex based on MALDI-TOF MS according to claim 3, wherein TA30 is acetonitrile mixed with ultrapure water containing 0.1% trifluoroacetic acid at a volume ratio of 30:70.
  5. 5. The method for detecting lanthanide metal-1, 3-dione complex based on MALDI-TOF MS according to claim 1, wherein the lanthanide metal-1, 3-dione complex is ytterbium tris (2, 6-tetramethyl-3, 5-heptanedionate) or cerium tetrakis (2, 6-tetramethyl-3, 5-heptanedionate) (IV).
  6. 6. The method for detecting lanthanide metal-1, 3-dione complex based on MALDI-TOF MS according to claim 2, wherein the solvent in the solution of lanthanide metal-1, 3-dione complex is chloroform.
  7. 7. The method for detecting lanthanide metal-1, 3-dione complex based on MALDI-TOF MS according to claim 2, wherein the lanthanide metal-1, 3-dione complex solution and the DHB matrix solution are mixed at a volume ratio of 1:1.
  8. 8. The method for detecting lanthanide metal-1, 3-dione complex based on MALDI-TOF MS according to claim 2, wherein the error between the [ M+K ] + mass spectrum result of the obtained lanthanide metal-1, 3-dione complex and the theoretical value is less than 5ppm.
  9. 9. The method for detecting lanthanide metal-1, 3-dione complex based on MALDI-TOF MS according to claim 1, wherein the lanthanide metal-1, 3-dione complex is tetrakis (2, 6-tetramethyl-3, 5-heptanedionato) cerium (IV) or tris (2, 6-tetramethyl-3, 5-heptanedionato) ytterbium.

Description

Lanthanide metal-1, 3-diketone complex detection method based on MALDI-TOF MS Technical Field The application relates to the technical field of lanthanide metal-1, 3-diketone complex detection, in particular to a detection method of lanthanide metal-1, 3-diketone complex based on MALDI-TOF MS. Background The lanthanide metal-1, 3-diketone complex is a metal-organic complex formed by chelating lanthanide metal cations and deprotonated anions with a 1, 3-diketonate structure through coordination bonds. There is a need in the art to obtain the relative molecular mass and high resolution isotope distribution results of such compounds in order to perform accurate structural validation, purity identification and property prediction of such species. At present, mass spectrometry detection of lanthanide metal-1, 3-diketone complexes is post-resolution detection, mass spectrometry detection of lanthanide metal cations is mostly an inductively coupled plasma mass spectrometry technology, anions with 1, 3-diketonate structures can be detected through electrospray mass spectrometry in a negative mode, and the combination of the two detection means can provide effective basis for mass spectrometry identification of lanthanide metal-1, 3-diketone complexes. But mass spectrum identification results of the substances cannot be obtained by only detecting by electrospray mass spectrum or inductively coupled plasma mass spectrum. However, the detection method has the advantages of long operation time, complicated steps, more needed instruments and incapability of obtaining two kinds of information, namely accurate relative molecular mass and high-resolution isotope distribution result, through one-time detection. In the literature, DART-MS mass spectrometry detection methods are also reported, and can be used for mass spectrometry detection of lanthanide metal-1, 3-dione complexes, but are limited by instrument factors, and few application examples are supported by only one paper. Among various mass spectrometry detection means, matrix assisted laser desorption time of flight mass spectrometry (MALDI-TOF MS) is widely used for mass spectrometry of macromolecules such as polysaccharides, proteins and polymers with high resolution and high sensitivity. The detection method is not found to be used for detecting lanthanide metal-1, 3-dione complexes. MALDI-TOF MS has not been shown to be useful for detecting lanthanide metal-1, 3-dione complexes. The information disclosed in the background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art. Disclosure of Invention Aiming at the technical problems, the application provides a lanthanide metal-1, 3-diketone complex detection method based on MALDI-TOF MS, which utilizes MALDI-TOF MS to realize high-resolution mass spectrum detection of the lanthanide metal-1, 3-diketone complex and provides a simpler, more convenient and effective means for mass spectrum analysis detection of the lanthanide metal-1, 3-diketone complex with low cost. The application provides a detection method of lanthanide metal-1, 3-diketone complex based on MALDI-TOF MS, which comprises the following steps: after a detection sample of the lanthanide metal-1, 3-diketone complex is prepared, reflection mode detection is adopted, the laser intensity is 45-55%, the voltage multiple is 13.9×, and detection is carried out by MALDI-TOF MS after sample application under the room temperature condition to obtain the relative molecular mass and isotope distribution result. Preferably, the preparation of the test sample comprises the steps of: dissolving lanthanide metal-1, 3-diketone complex to obtain lanthanide metal-1, 3-diketone complex solution; uniformly mixing lanthanide metal-1, 3-diketone complex solution and DHB matrix solution to obtain a detection sample; The concentration of the lanthanide metal-1, 3-dione complex solution in the test sample was 1 mg/mL. Preferably, the formulation of the DHB matrix solution comprises the steps of: the solution was dissolved in TA30 as a solvent, and a sodium chloride solution having a concentration of 0.5 mM and a potassium chloride solution having a concentration of 0.5 mM were added to prepare a DHB base solution having a concentration of 20 mg/mL. Preferably, TA30 is acetonitrile and 0.1% trifluoroacetic acid in ultrapure water at a volume ratio of 30:70. Preferably, the lanthanide metal-1, 3-dione complex is ytterbium tris (2, 6-tetramethyl-3, 5-heptanedionate) or cerium tetrakis (2, 6-tetramethyl-3, 5-heptanedionate) (IV). Preferably, the solvent in the lanthanide metal-1, 3-dione complex solution is chloroform. Preferably, the lanthanide metal-1, 3-dione complex solution is mixed with the DHB matrix solution in a volume ratio of 1:1. Preferably, the resulting [ M+K ]