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Method for determining content of impurities in linagliptin raw material

A technology of impurity content and API, applied in the field of biomedicine, can solve the problems affecting the quality of linagliptin products and the efficacy of linagliptin, and achieve the effects of quality control, good separation, and real measurement.

Active Publication Date: 2018-04-03
SUNSHINE LAKE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, in the production process of linagliptin raw materials, impurities such as synthetic starting materials and intermediates will be introduced, which will affect the quality of linagliptin products and the curative effect of linagliptin

Method used

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  • Method for determining content of impurities in linagliptin raw material
  • Method for determining content of impurities in linagliptin raw material
  • Method for determining content of impurities in linagliptin raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] In this example, the inventors introduced in detail the development process of the method for determining the impurity content in linagliptin bulk drug.

[0058] 1.1 Determination of buffer salt type and pH value

[0059] Linagliptin contains a primary amino group, and the CAD software predicts that the pKa of its conjugate acid is as high as 10.0, which is relatively strong; Linagliptin also contains multiple basic groups, all of which are connected with more complex groups. It is difficult to judge the acidity and alkalinity. It is necessary to select a buffer with an appropriate pH value to ensure that the compound to be separated exists in a single form during the separation process, so as to achieve the separation effect of a single peak, a sharp peak shape, and a reproducible retention time. Therefore, in the initial stage of method development, the inventors investigated the separation effect of linagliptin and corresponding impurities under the same gradient and ...

Embodiment 2

[0086] In this example, the inventor investigated the system applicability and sensitivity of the method for determining the impurity content in Linagliptin bulk drug determined in Example 1, and introduced in detail how to use the chromatographic conditions determined in Example 1 The obtained chromatograms were used to calculate the impurity content.

[0087] 2.1 Preparation of relevant solutions

[0088] The diluent (blank solution) is: acetonitrile: phase A = 1:4 mixed solution;

[0089] Test solution: Take about 20 mg of the test product, weigh it accurately, put it in a 100 mL volumetric flask, dissolve it with an appropriate amount of diluent, sonicate and dilute to the mark, shake well, and prepare 2 parts in parallel;

[0090] System suitability solution: Take about 4 mg of impurity A reference substance, weigh it into a 100mL volumetric flask, accurately pipette 5mL of the test solution 1 into the same 100mL volumetric flask, add diluent to dissolve and dilute to th...

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Abstract

The invention provides a method for determining content of impurities in a linagliptin raw material. The method comprises the steps as follows: analyzing the linagliptin raw material with HPLC (high performance liquid chromatography) to obtain a chromatogram; determining the content of impurities in the linagliptin raw material on the basis of the chromatogram, wherein the HPLC adopts the following conditions: a chromatographic column is a chromatographic column YMC-PACK ODS-AM with the specification of 4.6*250 mm and 5 mu m, a detector is (diode array detector) DAD, the detection wavelength is 226 nm, the column temperature is 25 DEG C, a mobile phase A is a 10 mmol / L potassium dihydrogen phosphate buffer solution with the pH in a range of 3.0-5.0, a mobile phase B is acetonitrile, the flow speed is 1.0 mL / min, operation lasts for 10 min, and the elution gradient is shown in the description. With the adoption of the detection method, the content of impurities in the linagliptin raw material can be determined conveniently, accurately and sensitively, so that the quality of the linagliptin raw material can be effectively controlled.

Description

technical field [0001] The invention relates to the field of biomedicine, in particular, the invention relates to a method for measuring the impurity content in linagliptin bulk drug. Background technique [0002] Type II diabetes is caused by insufficient secretion of insulin by the body's pancreatic beta cells or the insensitivity of target cells to insulin (insulin resistance), also known as non-insulin-dependent diabetes. Type II diabetes mostly occurs after the age of 35 to 40, accounting for more than 90% of diabetic patients. [0003] Linagliptin is an inhibitor of dipeptidyl peptidase-4 (DPP-4), and is an effective drug for treating type II diabetes. Its molecular structure is: It is easily soluble in methanol, slightly soluble in acetonitrile, and hardly soluble in water. [0004] However, in the production process of linagliptin API, impurities such as synthetic starting materials and intermediates will be introduced, which will affect the quality of linaglipti...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34G01N30/26
CPCG01N30/02G01N30/26G01N30/34
Inventor 舒伟虎杨成刘国柱
Owner SUNSHINE LAKE PHARM CO LTD
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