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Analysis method for impurity content of exenatide

A technology of exenatide and analysis method, applied in the field of analysis of exenatide impurity content

Inactive Publication Date: 2019-01-18
QILU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] The present invention provides a method for effectively separating and accurately quantifying specific impurities of exenatide, aiming at solving the problem of exenatide and its specific impurities [D-His 1 ]-Exenatide, [Double Pro 38 ]-Exenatide and [Des-Gly 2 Separation and Quantitative Determination of ]-Exenatide

Method used

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  • Analysis method for impurity content of exenatide
  • Analysis method for impurity content of exenatide
  • Analysis method for impurity content of exenatide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] Embodiment 1: ([D-His 1 ]-Exenatide)

[0100] 1. Chromatographic conditions:

[0101] Instrument: High Performance Liquid Chromatography—UV Detector

[0102] Chromatographic column: strong cation exchange column [PolysulfoEthyl A TM (3μm, 4.6*100mm, 300A)]

[0103] Mobile phase: Potassium dihydrogen phosphate buffer (take 4.76g of potassium dihydrogen phosphate, add water 1000ml to dissolve. Phosphoric acid adjusts the pH value to 4.0)-acetonitrile (56.4:43.6)

[0104] Column temperature: 50°C. Wavelength: 214nm. Flow rate: 1.2ml / min. Injection: 40 μl.

[0105] 2. Validation of analytical methods

[0106] 1) Specificity

[0107] (1) Blank solvent: Take 15ml of 1% ammonium bicarbonate solution, put it in a 50ml measuring bottle, add 1.5ml of trypsin solution, mix well, heat in a 37°C water bath for 0.5h, let cool, add 5ml of dilute phosphoric acid solution, mix well, Add 15ml of 1% ammonium bicarbonate solution, mix well, add water to dilute to the mark, and ob...

Embodiment 2

[0140] 1. Chromatographic conditions:

[0141] Instrument: High Performance Liquid Chromatography—UV Detector

[0142] Chromatographic column: use octadecylsilane bonded silica gel as filler [X-TerraMSC18 (5.0μm, 4.6*150mm)]

[0143] Mobile phase: A: 0.1mol / L potassium chloride solution (take 7.4g of potassium chloride, add 1ml of triethylamine, add water to 1000ml, adjust pH to 2.7 with phosphoric acid)

[0144] B: Acetonitrile

[0145] gradient elution procedure

[0146]

[0147] Column temperature: 45°C. Wavelength: 214nm. Flow rate: 1.0ml / min. Injection: 80 μl.

[0148] 2. Validation of analytical methods:

[0149] 1) Specific solution

[0150] (1) Blank solvent: Take 15ml of 1% ammonium bicarbonate solution, put it in a 25ml measuring bottle, add 1.5ml of trypsin solution, vortex and mix, put it in a 37°C water bath and heat for 0.5h, then add 2ml of glacial acetic acid to terminate the reaction, Add water to make up to the mark, shake well, and you get it.

...

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Abstract

The invention discloses an analysis method for impurity content of exenatide, and belongs to the technical field of medicine analysis. According to the method provided by the invention, the exenatideand three specific impurities are digested by using trypsin, after digestion, a sample is separately separated by using two chromatographic processes, impurity [D-His<1>]-exenatide, impurity [Double Pro<38>]-exenatide and impurity [Des-Gly<2>]-exenatide contents in the exenatide are computed and measured by using an external standard method. The method provided by the invention is convenient, efficient and high in accuracy, and can effectively separate impurities and accurately quantify the same.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to an analysis method for exenatide impurity content. The analytical method can easily separate and accurately quantify the three specific impurities of exenatide, which can be used as an important part of the quality control of exenatide. Background technique [0002] Exenatide is a polypeptide sequence containing 39 amino acids extracted from the venom of the American monitor lizard. It has 53% homology with GLP-1, and it shows stronger stability because it is not easy to be degraded by DPP-IV. sex and biological activity. Exenatide is a GLP-1 receptor agonist that can promote insulin secretion and is mainly used to improve blood sugar control in patients with type Ⅱ diabetes. [0003] Exenatide injection (Byetta, Byetta) jointly developed by Amylin Pharmaceutical Company (Amylin) and Eli Lilly and Company was launched in the United States in 2005, and long-act...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/02
CPCG01N30/06G01N30/02
Inventor 代连花赵慧英张磊张林
Owner QILU PHARMA CO LTD
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