A kind of high performance liquid chromatography detection method of chiral isomer content of ticagrelor
A high-performance liquid chromatography and chiral isomer technology, which is applied in the field of analysis and monitoring in medicinal chemistry, can solve problems such as unusable, short column life, long column equilibration time, etc., and achieve the effect of ensuring product quality and easy operation
Active Publication Date: 2018-08-31
CHENGDU XINJIE HIGH TECH DEV CO LTD
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Problems solved by technology
[0004] The molecular structure of ticagrelor contains 6 chiral carbon atoms, and impurities will be produced during the actual synthesis process and storage process, among which the chiral isomer impurity is one of the main impurities, and conventional analysis and detection methods are difficult Separation of numerous chiral isomeric impurities
There are existing literature or patent reports using cellulose (or polysaccharide derivatives) as fillers for the detection of chiral chromatographic columns, but they are all columns coated with cellulose (or polysaccharide derivatives) on the surface of silica gel. Long equilibration time, poor stability, poor reproducibility, short column life, and dichloromethane, chloroform and other solvents cannot be used as mobile phases
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Embodiment 1
[0054] Detection instrument: Shimadzu LC-2030 high performance liquid chromatography.
[0055] Chromatographic conditions: the chromatographic column is IC column (250 × 4.6mm, 5 μm), the column temperature is 25 ℃; using ultraviolet detector, the detection wavelength is set to 300nm; mobile phase flow rate is 1.0ml / min; with n-hexane-isopropanol-methanol (330 :15:15) is mobile phase A, with dichloromethane as mobile phase B, and the elution conditions are as shown in Table 3 below:
[0056] The elution condition of table 3 embodiment 1
[0057]
[0058]
[0059] Experimental steps:
[0060] Take an appropriate amount of ticagrelor sample, add absolute ethanol to dissolve and dilute to make a solution containing about 1 mg ticagrelor per 1 ml, as the test solution; measure an appropriate amount of the test solution, dilute it with absolute ethanol to prepare A solution containing about 1 μg ticagrelor per 1 ml was used as the control solution; another chiral isomer r...
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Abstract
The invention discloses a high performance liquid chromatography detection method of the content of chiral isomers of ticagrelor. The high performance liquid chromatography detection method takes cellulose-tri(3,5-dichlorophenylaminoformiate) bonded on the surface of silica gel as a chiral chromatographic column of a filling agent, takes a mixed solution of alkane-low carbon alcohol as a mobile phase A and takes dichloromethane and / or chloroform as a mobile phase B. The cellulose-tri(3,5-dichlorophenylaminoformiate) bonded on the surface of the silica gel is used as the chiral chromatographic column of the filling agent and the suitable mobile phase is used for carrying out gradient elution; all chiral isomer impurities of ticagrelor are rapidly and effectively separated in one step and an effective detection method is provided for detecting and controlling the isomers of ticagrelor, so that the product quality and drug safety of ticagrelor are guaranteed; a self contrast method is used for carrying out quantitative determination of the impurities and the detection method is simple and convenient to operate and low in detection cost, and has good flexibility, linearity, specificity, precision, accuracy, stability and durability; and the detection method is an effective detection method of the content of the isomers.
Description
technical field [0001] The invention belongs to the technical field of analysis and monitoring in medicinal chemistry, and more specifically relates to a high performance liquid chromatography detection method for the content of chiral isomers of ticagrelor. Background technique [0002] Ticagrelor (ticagrelor) is a new type of selective small molecule anticoagulant drug developed by AstraZeneca, and its chemical structure is shown in formula 1 below: [0003] [0004] The molecular structure of ticagrelor contains 6 chiral carbon atoms, and impurities will be produced during the actual synthesis process and storage process, among which the chiral isomer impurity is one of the main impurities, and conventional analysis and detection methods are difficult Separation of numerous chiral isomer impurities. There are existing literature or patent reports using cellulose (or polysaccharide derivatives) as fillers for the detection of chiral chromatographic columns, but they ar...
Claims
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IPC IPC(8): G01N30/74G01N30/60G01N30/06
CPCG01N30/06G01N30/60G01N30/74
Inventor 欧世荣李敏许娟马欢
Owner CHENGDU XINJIE HIGH TECH DEV CO LTD