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Method for determining trelagliptin related substances

A technology related to substances and mobile phases, which is applied in the field of chemical analysis, can solve the problems of no pharmacopoeia-listed troxagliptin succinate and no documentation, and achieve the effects of controllable related substances, scientific methods, and improved safety

Active Publication Date: 2018-10-19
NANJING VARSAL MEDICINE TECH DEV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there is no pharmacopoeia for the analysis of related substances of trexagliptin succinate, and there is no document providing high performance liquid chromatography for the determination of related substances of troxagliptin succinate

Method used

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  • Method for determining trelagliptin related substances
  • Method for determining trelagliptin related substances
  • Method for determining trelagliptin related substances

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0054] The present embodiment provides a method for determining related substances of trexagliptin, comprising the following steps:

[0055] S1. Preparation of the test solution;

[0056]Take trexagliptin, add solvent to dissolve and dilute to make the solution that contains succinate trexagliptin 1.0mg in every 1ml, as need testing solution; A solution containing 10 μg of trexagliptin succinate in 1 ml was used as a control solution. Inject the sample and record the chromatogram.

[0057] WelchUltimate AQ-C18 chromatographic column is obtained by using octadecylsilane bonded silica gel as the chromatographic column filler and filling it into the chromatographic column, and then loading and eluting. Wherein mobile phase A is phosphoric acid aqueous solution (take 1000ml of water, add phosphoric acid 1ml, pH value is 2.1), mobile phase B is acetonitrile; Flow rate: 1.0ml / min; Carry out linear gradient elution according to Table 3. For test results, see figure 1 and figure...

Embodiment 2-3

[0062] Need testing solution preparation is consistent with embodiment 1. Chromatographic conditions: mobile phase A is phosphoric acid aqueous solution (embodiment 2-0.09% phosphoric acid aqueous solution, embodiment 3-0.11% phosphoric acid aqueous solution), mobile phase B is acetonitrile; Flow rate: 1.0ml / min; Carry out linear gradient as listed in table 3 elute.

[0063] Embodiment 2 result sees attached image 3 and Figure 4 ; Embodiment 3 results are attached Figure 5 and 6 . pass image 3 , Figure 4 , Figure 5 and Figure 6 It can be seen that the condition of 0.1% phosphoric acid aqueous solution provided by the present application can meet the detection requirements, and the separation effect is good.

Embodiment 4-5

[0065] Need testing solution preparation is consistent with embodiment 1. Chromatographic conditions: mobile phase A is 0.1% phosphoric acid aqueous solution, mobile phase B is acetonitrile, the mobile phase of initial ratio (embodiment 4 initial ratio of acetonitrile is 13%, embodiment 5 initial ratio of acetonitrile is 17%); Flow velocity: 1.0ml / min; Example 4 was used for linear gradient elution in Table 4, and Example 5 was used for linear gradient elution in Table 4.

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Abstract

The invention relates to the field of chemical analysis, and particularly relates to a method for determining trelagliptin related substances. The method for determining trelagliptin related substances comprises the following steps: using octadecylsilane bonded silica gel as a chromatographic column filler and sampling a test article solution; then carrying out elution by using an acid solution asa flow phase A and an organic solvent as a flow phase B and carrying out detection. The octadecylsilane bonded silica gel and the acid solution are selected as the flow phase A and the organic solvent is selected as the flow phase B, so that the trelagliptin related substances are conveniently separated and eluted, and impurities of trelagliptin is fully revealed, the trelagliptin related substances can be quickly detected, and the security of the product is improved. The method disclosed by the invention has the advantages of science and reliability, and moreover, the trelagliptin related substances can be controlled.

Description

technical field [0001] The invention relates to the field of chemical analysis, in particular to a method for determining related substances of trexagliptin. Background technique [0002] Trelagliptin Succinate, chemical name: (R)-2-((6-(3-aminopiperidin-1-yl)-3-methyl-2,4-dioxo- 3,4-Dihydropyrimidin-1(2H)-yl)methyl)-4-fluorobenzocyanosuccinate is a long-acting dipeptidyl peptidase IV (DPP-4) inhibitor, used For the treatment of type 2 diabetes. [0003] The composition of trexagliptin succinate API is clear, mainly including trexagliptin succinate and 8 related substances. It is very important to separate these 9 substances thoroughly and quickly. [0004] At present, there is no pharmacopoeia that includes the analysis method for related substances of trexagliptin succinate, and there is no literature that provides high performance liquid chromatography for the determination of related substances of troxagliptin succinate. Contents of the invention [0005] The invent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 孙孝金纪德胜张德伟扈田进孙珏
Owner NANJING VARSAL MEDICINE TECH DEV
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