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Use of a substituted cyclotetraphosphazene compound

A cyclotetraphosphazene and compound technology, applied in the field of mass spectrometry analysis, can solve the problems of low sensitivity, no application report of cyclotetraphosphazene compounds, and high application concentration

Active Publication Date: 2019-10-15
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are still some defects in this type of calibrator. For example, the mass spectrum peaks obtained by the Ultramark 1621 calibrator have a Gaussian distribution with an interval of 100 amu, which can only be used in the mass range from about m / z 900 to m / z 2100, "low end " and "high-end" ions are significantly less than those in the middle; Agilent's G1969-85000 mass spectrometry calibration solution can only be used in the mass range from about m / z 100 to m / z 2700; and the application concentrations of the above-mentioned calibration solutions are higher, Up to 0.05% (mass fraction), not easy to be eluted, the ion source is easily polluted, the sensitivity is low, and memory effects will occur
[0006] At present, there are relatively few research reports on cyclotetraphosphazenes, and there are no reports on the application of cyclotetraphosphazenes in mass spectrometry calibration, and there are no reports on the application of cyclotetraphosphazenes in mass spectrometry calibration.

Method used

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  • Use of a substituted cyclotetraphosphazene compound
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  • Use of a substituted cyclotetraphosphazene compound

Examples

Experimental program
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Effect test

Embodiment 1

[0201] Homosubstituted cyclotetraphosphazenes: 2,2,4,4,6,6,8,8-octa(2,2-difluoroethoxy)-2λ 5 ,4λ 5 ,6λ 5 ,8λ 5 - Preparation of cyclotetraphosphazene (SMS-0828):

[0202] Add 104g (0.5mol) of phosphorus pentachloride, 29.4g of ammonium chloride (0.55mol) and 200mL of tetrachloroethane into a 500mL three-necked flask, heat to 147°C and reflux for 7 hours under stirring, to complete the reaction, evaporate the tetrachloride under reduced pressure. Ethane, and the residue was recrystallized from petroleum ether to obtain white crystals, Octachlorocyclotetraphosphazene, 19g, yield: 8.1%, melting point: 123.4-124.3°C;

[0203] Add 5mL of 2,2-difluoroethanol into a 100mL three-neck flask, cool to 0°C in an ice-water bath, add 460mg (20mmol) sodium metal in batches under stirring, remove the ice-water bath, react at room temperature for 30 minutes, then heat and reflux for 2 hours to end the reaction. The excess 2,2-difluoroethanol was distilled off under reduced pressure, and th...

Embodiment 2

[0205] Homosubstituted cyclotetraphosphazenes: 2,2,4,4,6,6,8,8-octa(2,2,3,3-tetrafluoropropoxy)-2λ 5 ,4λ 5 ,6λ 5 ,8λ 5 - Preparation of cyclotetraphosphazene (SMS-1228):

[0206] Add 400mg NaH (60%) and 50mL dry toluene to a 100mL three-necked flask, under nitrogen protection, slowly add dropwise a solution of 1.32g (10mmol) 2,2,3,3-tetrafluoropropanol dissolved in 5mL dry toluene under stirring, After reacting at room temperature for 30 minutes, heat and reflux for 2 hours, cool the reaction solution to 50°C, add dropwise a solution of 464 mg (1 mmol) octachlorocyclotetraphosphazene dissolved in 5 mL of dry toluene, heat and reflux and stir for 5 hours to complete the reaction, and depressurize The toluene was evaporated, and 100 mL of diethyl ether was added to the residue, and the resulting diethyl ether mixture was washed with 2N dilute hydrochloric acid, water, and saturated NaCl solution successively, and then washed with anhydrous MgSO 4 After drying and removing th...

Embodiment 3

[0208] Preparation of heterogeneously substituted cyclotetraphosphazenes (SMS-132-232):

[0209] Add 360mg NaH (60%) and 50mL dry toluene to a 100mL three-necked flask, under nitrogen protection, slowly add 0.58g (4.4mmol) 2,2,3,3-tetrafluoropropanol and 1.02g (4.4mmol) 2 , 2,3,3,4,4,5,5- Octafluoropentanol dissolved in 5mL of dry toluene solution, reacted at room temperature for 30 minutes, heated to reflux for 2 hours, cooled the reaction solution to 50°C, added dropwise 464mg (1mmol ) Octachlorocyclotetraphosphazene dissolved in 5mL of dry toluene solution, heated to reflux and stirred for 5 hours to complete the reaction, evaporated the toluene under reduced pressure, added 100mL ether to the residue, and washed the obtained ether mixture with 2N dilute hydrochloric acid, water, , washed with saturated NaCl solution, anhydrous MgSO 4 After drying, the solvent was spun off, and the solid was purified by column chromatography to obtain a light yellow oily compound (SMS-132-...

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Abstract

The invention discloses application of substituted cyclotetraphosphazene compounds. The chemical structure of the substituted cyclotetraphosphazene compounds is as shown in formula I. The applicationis characterized in that at least one of the substituted cyclotetraphosphazene compounds as shown in the formula I is used as the mass spectrum calibrator for the mass spectrum calibration of variousdifferent ion sources under a positive-ion or negative-ion ionization mode. The substituted cyclotetraphosphazene compounds are good in mass spectrum response, high in sensitivity, low in isotope contribution, low in use amount, capable of avoiding the generation of a memory effect, wide in applicable m / z range, nontoxic, odorless, stable, low in cost, quite good in popularization and applicationvalue and the like.

Description

technical field [0001] The invention relates to the use of a substituted cyclotetraphosphazene compound, which belongs to the technical field of mass spectrometry. Background technique [0002] Mass spectrometry is one of the most beneficial tools for substance identification. In order to obtain the accuracy and reliability of the identification results, it is often necessary to calibrate the mass spectrometer during the analysis and identification process. Mass spectrometry calibrators Highly accurate mass reference peaks are important for mass spectrometry because any calibration errors can be magnified and lead to a significant loss of precision. [0003] There are many kinds of mass spectrometry calibrators, including peptides, proteins, and some synthetic polymers, etc. These calibrators still have many limitations. For example: most calibrators can only be used to calibrate mass spectrometers in a specific mass-charge (m / z) range, and cannot be used to calibrate a wid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/62C07F9/6581
Inventor 郭寅龙曹瑾张芳刘素红张立张菁
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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