Method for analyzing and determining 2-(dibromo methyl)-4-fluorobenzonitrile in trelagliptin succinate

A technology of troxagliptin succinate and dibromomethyl, which is applied in the field of medicine and can solve the problem of no genotoxic impurities of troxagliptin succinate

Active Publication Date: 2019-04-23
浙江华贝药业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented process can detect small amounts (up to 1-6 ppb), but this technology works well only with certain types or sources of drug substances like tampered chlorpheniramine. It does provide technical benefits such as high accuracy and ease of operation compared to existing methods used by researchers working on chemicals produced from these compounds.

Problems solved by technology

This patented technical problem addressed in this patent relates to reducing certain substances called dopaminokine receptor proteins or transporters like neuropeptides GLUT1 , GTP, gamma amylincnecrosis protein 3, adenoscytoxy cyclodinucleotide pyridinetrone-5'-phosphate guided into cells through specific pathways involved in metabolism processes. These compound particles may lead to various diseases associated therewith including Parkinson' s disease, Type II Diabetes Mellitis, Syndrome X, Gastroparathormis Disorder, etc., which affect human health at least temporarily due to their ability to lower down excess amounts of harmful ingredients produced from gut hormones.

Method used

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  • Method for analyzing and determining 2-(dibromo methyl)-4-fluorobenzonitrile in trelagliptin succinate
  • Method for analyzing and determining 2-(dibromo methyl)-4-fluorobenzonitrile in trelagliptin succinate
  • Method for analyzing and determining 2-(dibromo methyl)-4-fluorobenzonitrile in trelagliptin succinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1 Specificity and Impurity Location Test

[0034] (1) Preparation of sample solution

[0035] Solvent: 50% acetonitrile aqueous solution

[0036] Positioning solution: troxagliptin succinate, 2-(dibromomethyl)-4-fluorobenzonitrile, 2-bromomethyl-6-fluorobenzonitrile, each appropriate amount, accurately weighed, and placed in different measuring bottles. , Add solvent (50% acetonitrile aqueous solution) to dissolve and dilute to prepare 6.67 containing troxagliptin succinate, 2-(dibromomethyl)-4-fluorobenzonitrile, 2-bromomethyl-6-fluorobenzonitrile each mg / ml, 1mg / ml, and 1ug / ml solutions are used as compound positioning solutions.

[0037] Specific solution: Take 10mg of 2-(dibromomethyl)-4-fluorobenzonitrile, accurately weigh it, place it in a 10ml measuring flask, add a solvent (50% acetonitrile aqueous solution) to dissolve and dilute to the 10ml mark, shake well. Take 100ul of the above solution in a 100ml volumetric flask, mix it with the diluent and make the vo...

Embodiment 2

[0053] Example 2 Detection limit and quantification limit

[0054] (1) Preparation of sample solution

[0055] Solvent: 50% acetonitrile aqueous solution

[0056] Measurement of baseline noise: accurately measure 10 μl of the solvent, inject it into the liquid chromatograph, and continuously inject 3 needles, and detect according to the chromatographic conditions described in the embodiment of the present invention. Record the blank baseline noise within the peak time range of 2-(dibromomethyl)-4-fluorobenzonitrile, and calculate the average value.

[0057] Preparation of quantification limit solution: Take appropriate amount of hetero-2-(dibromomethyl)-4-fluorobenzonitrile, accurately weigh, dissolve with solvent and gradually dilute, and detect according to the chromatographic conditions described in the embodiment of the present invention until it is diluted to The ratio of the peak height of 2-(dibromomethyl)-4-fluorobenzonitrile to the corresponding noise (ie signal-to-noise rat...

Embodiment 3

[0065] Example three linear

[0066] (1) Preparation of sample solution

[0067] Precisely weigh each 10mg of 2-(dibromomethyl)-4-fluorobenzonitrile, place it in a 100ml measuring flask, add solvent to dissolve and dilute to the mark, shake well; accurately measure 1ml, place it in a 100ml measuring flask, add Dilute the solvent to the mark, shake well, and use it as a linear stock solution.

[0068] Precisely measure 0.5ml, 1.5ml, 2.5ml, 4.0ml, 5.0ml, 6.0ml, 7.5ml of linear stock solution, put them in different 50ml measuring flasks, add solvent to dilute to the mark, shake well, respectively as the limit of 10 %, 30%, 50%, 80%, 100%, 120%, 150% linear solution. According to the chromatographic conditions of the present invention, linear equations and correlation coefficients are calculated.

[0069] (2) Chromatographic conditions

[0070] Chromatographic conditions are the same as in Example 1

[0071] (3) Experimental results

[0072] The test results show that 2-(dibromomethyl)-4-f...

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Abstract

The invention provides a method for analyzing and determining a genotoxic impurity 2-(dibromo methyl)-4-fluorobenzonitrile in trelagliptin succinate by utilizing HPLC (High Performance Liquid Chromatography). According to the method provided by the invention, an HPLC analysis method established by adopting octadecyl silane bonded silica gel as a stationary phase and a phosphoric acid water solution and an acetonitrile solution as moving phases and adopting a gradient eluting mode is capable of accurately determining the potential genotoxic impurity 2-(dibromo methyl)-4-fluorobenzonitrile in the trelagliptin succinate. An HPLC-UV (Ultraviolet) method is simple in operation, short in analysis time, high in accuracy degree and good in repeatability, the sensitivity can be up to 1.66ppm, a reliable detecting method is provided for quality standard of the trelagliptin succinate, safeguard is provided for health administration of a patient, and the method belongs to the technical field of medicine.

Description

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Claims

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Application Information

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Owner 浙江华贝药业有限责任公司
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