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Method for separating and detecting 4, 5, 6, 7-tetrahydrothiophene [3, 2-c] pyridine hydrochloride and related substances thereof

A technology of pyridine hydrochloride and tetrahydrothiophene, which is applied in the direction of material separation, measuring devices, and analysis materials, can solve the problems of unspecified gradient elution procedures, separation, etc., and achieve excellent ultraviolet absorption, good peak shape, The effect of high sensitivity

Active Publication Date: 2021-06-15
WUHAN WUYAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are no relatively mature reports on the analysis and detection of 4,5,6,7-tetrahydrothiophene[3,2-c]pyridine hydrochloride
Prior art: "Science Technology and Engineering Volume 13 No. 30 (Synthesis of 4,5,6,7-tetrahydrothieno[3,2-c]pyridine)" discloses gradient elution for HPLC method , but the gradient elution procedure was not specified in the literature, and 4,5,6,7-tetrahydrothiophene[3,2-c]pyridine hydrochloride could not be completely separated from its related substances by using the literature method

Method used

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  • Method for separating and detecting 4, 5, 6, 7-tetrahydrothiophene [3, 2-c] pyridine hydrochloride and related substances thereof
  • Method for separating and detecting 4, 5, 6, 7-tetrahydrothiophene [3, 2-c] pyridine hydrochloride and related substances thereof
  • Method for separating and detecting 4, 5, 6, 7-tetrahydrothiophene [3, 2-c] pyridine hydrochloride and related substances thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1: Separation and detection of 4,5,6,7-tetrahydrothiophene[3,2-c]pyridine hydrochloride and its related substances

[0050] This example provides a method for the separation and detection of 4,5,6,7-tetrahydrothiophene[3,2-c]pyridine hydrochloride and its related substances by high performance liquid chromatography, the method comprising the following steps:

[0051] 1) Weigh 20 mg of 4,5,6,7-tetrahydrothiophene[3,2-c]pyridine hydrochloride sample, put it in a 100ml volumetric flask, add mobile phase to dissolve and dilute to the mark, shake well, and use it as a sample solution;

[0052] 2) Take the sample solution, carry out HPLC analysis according to the following chromatographic conditions, and record the chromatogram;

[0053] Chromatographic conditions:

[0054] High-performance liquid chromatography: Dianne: UltiMate3000;

[0055] Column: Welch XB-C18 (250mm×4.6mm, 5μm);

[0056] Mobile phase: acetonitrile: 25mmol / L potassium dihydrogen phosphate bu...

Embodiment 2

[0063] In this example, the separation and detection of 4,5,6,7-tetrahydrothiophene[3,2-c]pyridine hydrochloride and its related substances are carried out according to the same method as in Example 1. The only difference is that the The column temperature was 35°C.

[0064] figure 2 The HPLC chart when the column temperature is 35°C, figure 2 Peak No. 1 is impurity A, peak No. 2 is 4,5,6,7-tetrahydrothiophene[3,2-c]pyridine hydrochloride, peak No. 3 is 2-thiopheneethylamine, and peak No. 4 is impurity C, peak No. 5 is impurity B, peak No. 6 is impurity D. It can be seen that under this condition 4,5,6,7-tetrahydrothiophene[3,2-c]pyridine hydrochloride main peak can be well separated from raw materials and impurities, and 4,5,6,7-tetrahydrothiophene The main peak of [3,2-c]pyridine hydrochloride is around 9.7min.

Embodiment 3

[0066] In this example, the separation and detection of 4,5,6,7-tetrahydrothiophene[3,2-c]pyridine hydrochloride and its related substances are carried out according to the same method as in Example 1. The only difference is that the The flow rate of the mobile phase is: 1.0ml / min.

[0067] image 3 The HPLC figure when the mobile phase flow rate is 1.0ml / min, image 3 Peak No. 1 is impurity A, peak No. 2 is 4,5,6,7-tetrahydrothiophene [3,2-c] pyridine hydrochloride, peak No. 3 is 2-thiopheneethylamine + impurity C, peak No. 4 The peak is impurity B, and the peak No. 5 is impurity D. It can be seen that under this condition 4,5,6,7-tetrahydrothiophene[3,2-c]pyridine hydrochloride main peak cannot achieve good separation with raw materials and impurities, and 4,5,6,7-tetrahydro The main peak of thiophene[3,2-c]pyridine hydrochloride is around 5.7min.

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Abstract

The invention discloses a method for separating and detecting 4, 5, 6, 7-tetrahydrothiophene [3, 2-c] pyridine hydrochloride and related substances thereof through high performance liquid chromatography. The method comprises the following steps of: 1) preparing a sample solution, specifically, taking a 4, 5, 6, 7-tetrahydrothiophene [3, 2-c] pyridine hydrochloride sample, and dissolving the sample with a mobile phase to prepare a sample solution of 4, 5, 6, 7-tetrahydrothiophene [3, 2-c] pyridine hydrochloride; and 2) taking the sample solution, injecting the sample solution into a high performance liquid chromatograph, recording a chromatogram, and completing separation and detection of the 4, 5, 6, 7-tetrahydrothiophene [3, 2-c] pyridine hydrochloride sample. In the high performance liquid chromatography, the mobile phase comprises an organic phase and a 25 mmol / L monopotassium phosphate buffer solution, and the volume ratio of the organic phase to the 25 mmol / L monopotassium phosphate buffer solution is (25: 75)-(5: 95), wherein the organic phase is methanol or acetonitrile. The method provided by the invention can be used for effectively separating the 4, 5, 6, 7-tetrahydrothiophene [3, 2-c] pyridine hydrochloride and related substances thereof, so that the quality control of raw material medicines and preparations of platelet coagulation inhibitor medicines is realized.

Description

technical field [0001] The invention relates to the technical field of compound detection, in particular to a method for separating and detecting 4,5,6,7-tetrahydrothiophene[3,2-c]pyridine hydrochloride and related substances thereof by high performance liquid chromatography. Background technique [0002] 4,5,6,7-Tetrahydrothieno[3,2-c]pyridine hydrochloride is a pharmaceutical intermediate, mainly used in the synthesis of platelet coagulation inhibitors such as ticlopydine, clopidogrel, prasugrel and other drugs. In order to improve the quality of pharmaceutical production, in accordance with pharmaceutical production specifications and product standards, such as the United States Pharmacopoeia (USP) and European Pharmacopoeia (EP), it is necessary to identify the key intermediate 4,5,6,7-tetrahydrothiophene [3,2 -c] pyridine hydrochloride quality for effective analysis and control, analysis of 4,5,6,7-tetrahydrothiophene [3,2-c] pyridine hydrochloride preparation and degr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/74
CPCG01N30/02G01N30/06G01N30/74
Inventor 赵涛涛黄婕冯路平王成张伟肖应国张琦
Owner WUHAN WUYAO PHARMA