Non-aqueous reversed-phase chromatographic detection method of borate compounds

A technology of borate esters and reversed-phase chromatography, which is applied in the field of liquid chromatography non-aqueous reversed-phase detection of borate compounds. Good shape, fast separation speed and high stability

Inactive Publication Date: 2018-06-08
CHANGZHOU HEQUAN PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a non-aqueous reversed-phase chromatographic detection method for borate compounds, so as to overcome the instability of borate compounds in the prior art when encountering water, which cannot be detected by ordinary reversed-phase liquid phase systems. The problem with testing

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  • Non-aqueous reversed-phase chromatographic detection method of borate compounds
  • Non-aqueous reversed-phase chromatographic detection method of borate compounds
  • Non-aqueous reversed-phase chromatographic detection method of borate compounds

Examples

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example 1

[0166] Example 1: The laboratory uses conventional reversed-phase liquid chromatography instrument Thermo U-3000, chromatographic grade solvent acetonitrile, tetrahydrofuran, etc., and uses Thermo Hypercarb (150mm*4.6mm, 5.0um) column for separation and analysis:

[0167] step one

[0168] Tetrahydrofuran acetonitrile is used as mobile phase, and acetonitrile is used as solvent to dissolve samples to detect stability;

[0169] step two

[0170] Reagents: tetrahydrofuran, acetonitrile (chromatographically pure), ultrapure water

[0171] Instrument: Thermo U-3000

[0172] Chromatographic column: Thermo Hypercarb (150mm*4.6mm, 5.0um)

[0173] Column temperature: 35°C

[0174] mobile phase:

[0175] Phase A: tetrahydrofuran

[0176] Phase B: Acetonitrile

[0177] Gradient program:

[0178] Time(min) A% B%

[0179] 0.00 10 90

[0180] 10.00 10 90

[0181] Flow rate: 1.0ml / min

[0182] Detector wavelength: UV 220nm

[0183] Injection volume: 5μl

[0184] Needle washing...

example 2

[0194] Example 2: The laboratory uses conventional reversed-phase liquid chromatography instrument Thermo U-3000, chromatographic grade solvent acetonitrile, tetrahydrofuran, etc., and uses Thermo Hypercarb (150mm*4.6mm, 5.0um) column for separation and analysis to optimize the compound of formula II.

[0195] step one

[0196] Dichloromethane and acetonitrile were used as mobile phase, and acetonitrile was used as solvent to dissolve the sample, and the stability was tested.

[0197] step two

[0198] Reagents: dichloromethane, acetonitrile (chromatographically pure), ultrapure water

[0199] Instrument: Thermo U-3000

[0200] Chromatographic column: Thermo Hypercarb (150mm*4.6mm, 5.0um)

[0201] Column temperature: 25°C

[0202] mobile phase:

[0203] Phase A: dichloromethane

[0204] Phase B: Acetonitrile

[0205] Gradient program:

[0206] Time(min) A% B%

[0207] 0.00 20 80

[0208] 10.00 20 80

[0209] Flow rate: 0.5ml / min

[0210] Detector wavelength: UV 230...

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Abstract

The invention discloses a non-aqueous reversed-phase chromatographic detection method of borate compounds. An organic solvent in a reversed-phase liquid phase system replaces the conventional aqueousphase, mobile phase components are all organic solvents, and the effective separation of borate compounds is realized through a conventional C18 or graphitized carbon chromatographic column in the isocratic or gradient mode. The borate compounds are pinacol borate lactone compounds which are five-membered lactone compounds obtained by condensation of monoboronic acid or substituted boronic acid and monopinacol. The method prevents the water instability of the borate compounds. Through use of different organic phase solutions as modifiers, the selectivity of different borate compounds is changed. The method can realize accurate qualitification and quantification, good peak shapes, a high separation degree, fastness, high efficiency and a stable compound separation environment.

Description

technical field [0001] The invention relates to a detection method in the field of analytical chemistry, in particular to a liquid chromatography non-aqueous reversed-phase detection method for borate compounds. Background technique [0002] Borate ester compounds were originally used as lubricating oil additives. With the rapid development of the pharmaceutical industry, borate esters, especially borate lactone compounds (such as boric acid pinacol lactone, etc.) have become key intermediates for many active pharmaceutical ingredients. It is applicable to various biological activities in medicine. For example, it selectively blocks the proliferation of tumor cells, induces apoptosis, and effectively inhibits the growth of human tumor cells. However, there are still many problems in the analysis method of borate drug intermediates. [0003] For example, boric acid esters are unstable when exposed to water, and the nature of their easy hydrolysis is because the boron atom i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 李进晨蓝仁青赵初芒蒋竞
Owner CHANGZHOU HEQUAN PHARMA CO LTD
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