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Method for analyzing and determining 2-cyano-5-fluorobenzyl bromide in trelagliptin succinate

A technology of troxagliptin succinate and fluorobenzyl bromide, which is applied in the field of medicine and can solve problems such as the absence of reports on the detection method of 2-cyano-5-fluorobromobenzyl

Pending Publication Date: 2020-07-28
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

Problems solved by technology

Currently, USP, EP, JP, Chinese Pharmacopoeia and related literatures and patents have no report on the detection method of trexagliptin succinate genotoxic impurity 2-cyano-5-fluorobenzyl bromide

Method used

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  • Method for analyzing and determining 2-cyano-5-fluorobenzyl bromide in trelagliptin succinate
  • Method for analyzing and determining 2-cyano-5-fluorobenzyl bromide in trelagliptin succinate
  • Method for analyzing and determining 2-cyano-5-fluorobenzyl bromide in trelagliptin succinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1 specificity and impurity localization test

[0034] (1) Preparation of sample solution

[0035] Solvent: 50% acetonitrile in water

[0036] Positioning solution: troxagliptin succinate, 2-cyano-5-fluorobenzyl bromide, 2-(dibromomethyl)-4-fluorobenzonitrile (the by-product of the synthesis of 2-cyano-5-fluorobenzyl bromide , is a genotoxic impurity) each appropriate amount, accurately weighed, put in different volumetric flasks respectively, and add solvent (50% acetonitrile aqueous solution) to dissolve and dilute to make trexagliptin containing succinate, 2-cyano-5-fluoro 6.67 mg / ml, 0.1 mg / ml, and 0.1 mg / ml solutions of benzyl bromide and 2-(dibromomethyl)-4-fluorobenzonitrile were used as compound localization solutions.

[0037] Specific solution: Weigh 10 mg of 2-cyano-5-fluorobenzyl bromide, weigh it accurately, put it in a 10 ml volumetric flask, dissolve it with a solvent (50% acetonitrile aqueous solution), and shake it up. Measure 100ul of the ...

Embodiment 2

[0052] Embodiment two detection limit and limit of quantification

[0053] (1) Preparation of sample solution

[0054] Solvent: 50% acetonitrile in water

[0055] Measurement of baseline noise: Precisely measure 10 μl of solvent, inject it into a liquid chromatograph, inject 3 needles continuously, and detect according to the chromatographic conditions described in the embodiment of the present invention. Record the blank baseline noise within the peak eluting time range of 2-cyano-5-fluorobenzyl bromide, and calculate the average value.

[0056] Preparation of limit of quantitation solution: Take an appropriate amount of 2-cyano-5-fluorobenzyl bromide, accurately weigh it, dissolve it with a solvent and gradually dilute it, and detect it according to the chromatographic conditions described in Example 1 of the present invention until it is diluted to 2-cyano- The peak height of 5-fluorobromobenzyl and the ratio of corresponding noise (i.e. signal-to-noise ratio, S / N) is abo...

Embodiment 3

[0064] Example Trilinear

[0065] (1) Preparation of sample solution

[0066] Accurately weigh 10mg of 2-cyano-5-fluorobenzyl bromide in a 100ml volumetric flask, dissolve it with diluent and constant volume, shake well; accurately measure 1ml of the above solution into a 100ml volumetric flask, add diluent to dissolve and constant volume, shake homogeneously, as a linear stock solution.

[0067] Accurately measure 1.5ml, 2.5ml, 4.0ml, 5.0ml, 6.0ml and 7.5ml of the linear stock solution respectively, place them in different 50ml volumetric flasks, dissolve them with the diluent and constant volume, shake well, and use them as the limit of 30ml respectively. %, 50%, 80%, 100%, 120%, 150% linear solution. According to the chromatographic conditions described in the present invention, the linear equation and the correlation coefficient are calculated.

[0068] (2) Chromatographic conditions

[0069] The chromatographic conditions are the same as in Example 1.

[0070] (3) Ex...

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Abstract

The invention provides a method for analyzing and determining 2-cyano-5-fluorobenzyl bromide in trelagliptin succinate. According to the method, octadecylsilane chemically bonded silica is adopted asa stationary phase, a phosphoric acid aqueous solution and an acetonitrile solution are adopted as mobile phases, a gradient elution mode is adopted, and an established high performance liquid chromatography method can accurately determine the potential genotoxic impurity 2-cyano-5-fluorobenzyl bromide in trelagliptin succinate. The HPLC-UV method is simple to operate, short in analysis time, highin accuracy and good in repeatability; the sensitivity of the method can reach 3.0 ppm; a reliable detection method is provided for the quality standard of trelagliptin succinate; a guarantee is provided for the healthy medication of patients; and the HPLC-UV method belongs to the technical field of medicines.

Description

technical field [0001] The invention belongs to the field of medicine, and specifically discloses a drug analysis method for determining the potential genotoxic impurity 2-cyano-5-fluorobenzyl bromide in trexagliptin succinate by using an HPLC method. Background technique [0002] Trelagliptin (Trelagliptin) is a once-weekly dipeptidyl peptidase IV (DPP-4) inhibitor that controls blood sugar levels through selective and sustained inhibition of DPP-4. DPP-4 is a serine protease that can trigger the inactivation of incretins (glucagon-like peptide-1 (GLP-1) and glucose-dependent insulinotropic polypeptide (GIP)), and these two incretins in blood glucose important role in regulation. Inhibition of DPP-4 can increase blood glucose level-dependent insulin secretion, thereby controlling blood glucose levels. For this medicine, the purity of its main components is the decisive factor for the efficacy of the medicine, so the subsequent detection of the preparation of the medicine ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 钱王科孙冰洋李成美王红燕郑文瑾
Owner 浙江华贝药业有限责任公司
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