Method for analyzing and detecting Prasugrel intermediate

A detection method and intermediate technology, applied in the field of high-performance liquid chromatography analysis, can solve the problems affecting the quality of the final product, difficult to separate, etc., and achieve the effect of stable and reliable results, high resolution, and quality assurance

Active Publication Date: 2015-01-14
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Due to the existence of this keto-enol tautomer, the prasugrel intermediate will appear double peaks in the liquid chromatogram, and it is difficult to separate. So far, USP, EP, BP, JP and Chinese Pharmacopoeia and The analysis and detection method of the prasugrel intermediate is not recorded in the patent literature, but the analysis and detection of the prasugrel intermediate plays an important role in the reaction control and yield improvement, and also directly affects the quality of the final product. A rapid and effective analytical detection method is very necessary for the quality control of prasugrel intermediates

Method used

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  • Method for analyzing and detecting Prasugrel intermediate
  • Method for analyzing and detecting Prasugrel intermediate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Instruments and conditions: Agilent1260 liquid chromatography system, DAD detector, chromatographic column: ZORBAX SB-C18 (150×4.6mm, 5μm); detection wavelength: 220nm; column temperature is room temperature; injection volume 20μL; flow rate 1.0mL / min ; With 0.1% phosphoric acid aqueous solution as mobile phase A and acetonitrile as mobile phase B, carry out gradient elution according to Table 1.

[0027] Table 1 Concentration gradient of mobile phase

[0028]

[0029] Experimental procedure: Dissolve the prasugrel intermediate with 60% acetonitrile aqueous solution and quantitatively dilute it to make a solution containing 0.4 mg of prasugrel intermediate per 1 ml as the test solution; accurately measure 20 μL of the test solution for injection Phase chromatograph, record chromatogram, see attached HPLC spectrum figure 1 .

[0030] Depend on figure 1 It can be seen that under this chromatographic condition, the retention times of the ketoenene tautomeric peaks A ...

Embodiment 2

[0032] Instruments and conditions: Agilent1260 liquid chromatography system, DAD detector, chromatographic column: ZORBAX SB-C18 (150×4.6mm, 5μm); detection wavelength: 220nm; column temperature is room temperature; injection volume 10μL; flow rate 1.0mL / min ; With 0.2% phosphoric acid aqueous solution as mobile phase A and acetonitrile as mobile phase B, carry out gradient elution according to Table 2.

[0033] Table 2 Concentration gradient of mobile phase

[0034]

[0035] Experimental procedure: Dissolve the prasugrel intermediate with 60% acetonitrile aqueous solution and quantitatively dilute it to make a solution containing 0.6 mg of prasugrel intermediate per 1 ml as the test solution; accurately measure 10 μL of the test solution for injection Phase chromatograph, record chromatogram, see attached HPLC spectrum figure 2 .

[0036] Depend on figure 2 It can be seen that under this chromatographic condition, the retention times of the ketoenene tautomeric peaks ...

Embodiment 3

[0038] Instruments and conditions: Agilent1260 liquid chromatography system, DAD detector, chromatographic column: ZORBAX SB-C18 (150×4.6mm, 5μm); detection wavelength: 220nm; column temperature is room temperature; injection volume 40μL; flow rate 1.1mL / min ; With 0.3% phosphoric acid aqueous solution as mobile phase A and acetonitrile as mobile phase B, carry out gradient elution according to Table 3.

[0039] Table 3 Concentration Gradient of Mobile Phase

[0040]

[0041] Experimental procedure: Dissolve the prasugrel intermediate with 60% acetonitrile aqueous solution and quantitatively dilute it to make a solution containing 0.3 mg of prasugrel intermediate per 1 ml as the test solution; accurately measure 40 μL of the test solution for injection Phase chromatograph, record chromatogram, see attached HPLC spectrum image 3 .

[0042] Depend on image 3 It can be seen that under this chromatographic condition, the retention times of the ketoenene tautomeric peaks A ...

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Abstract

The invention relates to a method for analyzing and detecting a Prasugrel intermediate. The method is used for quality control of 5-[2-cyclopropyl-1-(2-fluorophenyl)-2-oxoethyl]-5,6,7,7A-tetrahydrothieno[3,2-C]pyridine-2(4H)-one. The method realizes reversed phase high-performance liquid chromatography-based analysis and detection under the conditions of a chromatographic column (C18, 4.6*150mm, 5 microns) filled with octadecyl silane bonded silica gel which is used as a filling material, phosphoric acid aqueous solution-acetonitrile or acetic acid aqueous solution-acetonitrile as a mobile phase and detection wavelength of 220nm. The method has the advantages of high degree of separation, short analysis time, simple operation and stable and reliable analysis.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography analysis method, in particular to an analysis and detection method of a prasugrel intermediate. Background technique [0002] Prasugrel is a tetrahydrothienopyridine drug jointly developed by Sankyo Company of Japan and Eli Lilly Company of the United States. It has a similar structure to clopidogrel, but is superior to clopidogrel in terms of activity, tolerance and safety. Clinical studies have shown that patients taking prasugrel have a lower comprehensive risk of heart attack and stroke, and the effect is quick after taking the drug, the blood concentration is stable, and the effect is long-lasting. [0003] 5-[2-Cyclopropyl-1-(2-fluorophenyl)-2-oxoethyl]-5,6,7,7A-tetrahydrothieno[3,2-C]pyridine-2( 4H)-ketone is an important intermediate for the synthesis of prasugrel, and its molecular formula is C 18 h 18 FNO 2 S, molecular weight 331.40, structural formula as follows: [0004...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 赵志全
Owner LUNAN PHARMA GROUP CORPORATION
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