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Method for measuring related substances in succinic acid Trelagliptin raw materials

A technology of troxagliptin succinate and related substances, which is applied in the field of determination of related substances in trexagliptin raw materials, can solve problems such as impurity cannot be covered, applicability cannot be judged, quality control of this product cannot be guaranteed, and the quality can be achieved. control effect

Active Publication Date: 2016-06-22
中山万远新药研发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method has the following problems: 1. The patent does not give any known impurities, and the applicability of the method cannot be judged; 2. The wavelength parameter of the analysis method is set to 278nm, which cannot cover all impurities. Spectral analysis of impurities, impurity P does not have any UV absorption at 278nm
The above problems indicate that this analytical method cannot guarantee the quality control of this product

Method used

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  • Method for measuring related substances in succinic acid Trelagliptin raw materials
  • Method for measuring related substances in succinic acid Trelagliptin raw materials
  • Method for measuring related substances in succinic acid Trelagliptin raw materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Instruments and Experimental Conditions

[0057] High performance liquid chromatography: Shimadzu LC-20AD

[0058] Chromatographic column: 100-5C18 (Kromasil, 250×4.6mm, 5μm)

[0059] Mobile phase A is a mixed solution of 0.1% (v / v) perchloric acid aqueous solution: acetonitrile=90:10 (v / v) with triethylamine to adjust the pH value to 3.0, and mobile phase B is to use triethylamine to adjust the pH A mixed solution of 0.1% (v / v) perchloric acid aqueous solution with a value of 3.0: acetonitrile = 40:60 (v / v); gradient elution according to Table 2.

[0060]

[0061]

[0062] The flow rate is 1.0ml / min;

[0063] Column temperature 40°C;

[0064] Detection wavelength 224nm;

[0065] The injection volume was 10 μl.

[0066] Experimental steps:

[0067] Take the blank solution and the mixed impurity reference substance solution respectively, carry out high performance liquid chromatography analysis according to the above experimental conditions, and record the chr...

Embodiment 2

[0070] Instruments and Experimental Conditions

[0071] High performance liquid chromatography: Shimadzu LC-20AD

[0072] Chromatographic column: 100-5C18 (Kromasil, 250×4.6mm, 5μm)

[0073] Mobile phase A is a mixed solution of 0.1% (v / v) perchloric acid aqueous solution: acetonitrile=90:10 (v / v) with triethylamine to adjust the pH value to 3.0, and mobile phase B is to use triethylamine to adjust the pH A mixed solution of 0.1% (v / v) perchloric acid aqueous solution with a value of 3.0: acetonitrile = 40:60 (v / v); elution according to the linear gradient in Table 3.

[0074]

[0075]

[0076] The flow rate is 1.0ml / min;

[0077] Column temperature 40°C;

[0078] Detection wavelength 197nm, 224nm, 235nm;

[0079] The injection volume was 10 μl.

[0080] Experimental steps:

[0081] Get about 25 mg of trexagliptin succinate raw drug sample (WY022-12 batch), put it in a 50ml volumetric flask, dissolve the sample with a blank solution, and prepare a sample solution co...

Embodiment 3

[0084] Instruments and Experimental Conditions

[0085] High performance liquid chromatography: Shimadzu LC-20AD

[0086] Chromatographic column: 100-5C18 (Kromasil, 250×4.6mm, 5μm)

[0087] Mobile phase A is a mixed solution of 0.1% (v / v) perchloric acid aqueous solution: acetonitrile=90:10 (v / v) with triethylamine to adjust the pH value to 3.0, and mobile phase B is to use triethylamine to adjust the pH A mixed solution of 0.1% (v / v) perchloric acid aqueous solution with a value of 3.0: acetonitrile = 40:60 (v / v); elution according to the linear gradient in Table 4.

[0088]

[0089]

[0090] The flow rate is 0.8ml / min;

[0091] Column temperature 35°C;

[0092] Detection wavelength 197nm, 224nm, 235nm;

[0093] The injection volume was 10 μl.

[0094] Experimental steps:

[0095] Get about 25 mg of trexagliptin succinate bulk drug sample (WY022-12 batch), put in a 50ml volumetric flask, dissolve the sample with a blank solution, and prepare a sample solution cont...

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Abstract

The invention discloses a method for measuring related substances in succinic acid Trelagliptin raw materials and relates to the field of analytic chemistry. According to the method, high performance liquid chromatography is adopted, a sample solution is injected into a high performance liquid chromatograph, and the related substances in the succinic acid Trelagliptin raw materials are measured; according to chromatographic conditions, a 100-5C18 chromatographic column of the Kromasil company is adopted as a chromatographic column, a flowing phase A and a flowing phase B are both a mixed solution of an acid aqueous solution and an organic solvent, the sum of the volume percentage of the flowing phase A and the volume percentage of the flowing phase B is kept 100% all the time, and linear gradient elution is performed. According to the method, the 100-5C18 chromatographic column of the Kromasil company is adopted, the gradient elution program of the flowing phases is optimized, and the related substances in the succinic acid Trelagliptin raw materials can be effectively separated. The method solves the separation and measurement problem of the related substances in the succinic acid Trelagliptin raw materials, and therefore it is guaranteed that the mass of the succinic acid Trelagliptin raw materials is controllable.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for determining related substances in trexagliptin raw materials. Background technique [0002] Among the antidiabetic drugs, the research of orally administered small molecule DPP-IV inhibitors is the most active. DPP-IV is an enzyme in the body that triggers the inactivation of incretins, glucone-like peptide-1 and glucose-dependent insulinotropic polypeptide, two incretins that play an important role in blood glucose regulation . Inhibition of DPP-IV can increase blood glucose level-dependent insulin secretion, thereby controlling blood glucose levels. [0003] DPP-IV inhibitor drugs are named "gliptins". There are 17 such drugs. Among them, trexagliptin was developed by Takeda Pharmaceutical and was first approved for marketing in Japan in 2014. It is an ultra-long-acting The DPP-IV inhibitor only needs to be taken orally once a week, which can produce continuo...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/065
Inventor 王佳平王鹤然杜志博陈嘉智邵施雅彭韪
Owner 中山万远新药研发有限公司
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