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Method for detecting peramivir intermediate I by reversed-phase high performance liquid chromatography

A reversed-phase high-performance liquid phase, chromatographic detection technology, applied in the field of reversed-phase high-performance liquid chromatography detection of peramivir trihydrate intermediate I, can solve the problems affecting the quality of peramivir and drug safety, quality differences Large size, difficulty in mobile phase pH screening, etc., to achieve the effects of short detection time, accurate detection and quality control, and guaranteed specificity

Active Publication Date: 2021-05-25
日照正济药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are many manufacturers supplying peramivir intermediates in the market, and the quality varies greatly. There are some impurity compounds. The existence of some impurities will seriously affect the quality and drug safety of peramivir, so it needs to be tested and quality controlled.
There are multiple pKa's in the intermediate of peramivir, which makes it difficult to screen the pH of the mobile phase

Method used

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  • Method for detecting peramivir intermediate I by reversed-phase high performance liquid chromatography
  • Method for detecting peramivir intermediate I by reversed-phase high performance liquid chromatography
  • Method for detecting peramivir intermediate I by reversed-phase high performance liquid chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1: specificity test

[0039] Diluent: Methanol

[0040] Impurity 1 positioning solution: Take about 5 mg of the impurity 1 reference substance, weigh it accurately, put it in a 10ml measuring bottle, add diluent to dissolve and dilute to the mark and shake well to prepare a solution with a concentration of the impurity 1 reference substance of about 0.5 mg / ml.

[0041] Impurity 2 positioning solution: take about 5 mg of the impurity 2 reference substance, weigh it accurately, put it in a 10ml measuring bottle, add diluent to dissolve and dilute to the mark and shake well to prepare a solution with a concentration of the impurity 2 reference substance of about 0.5 mg / ml.

[0042] Impurity 3 positioning solution: Take about 5 mg of the impurity 3 reference substance, weigh it accurately, put it in a 10ml measuring bottle, add diluent to dissolve and dilute to the mark and shake well to prepare a solution with a concentration of the impurity 3 reference substanc...

Embodiment 2

[0055] Embodiment 2: sensitivity test

[0056] Take the system suitability solution prepared in Example 1 and dilute it step by step to an appropriate multiple. The solution with a signal-to-noise ratio ≥ 10:1 is used as the solution for the limit of quantification; the solution with a signal-to-noise ratio ≥ 3: 1 is used as the solution for the limit of detection.

[0057] Precisely measure 5 μl of each of the above solutions, inject them into the liquid chromatograph, continuously inject 6 injections of the limit of quantification solution, inject 1 injection of the detection limit solution, and record the chromatogram. The results are shown in Table 2.

[0058] Table 6 Quantitative limit, detection limit result

[0059]

[0060]

Embodiment 3

[0061] Embodiment 3: linearity test

[0062] Get the peramivir intermediate reference substance solution and dilute it with a diluent to make a series of concentration control solutions, inject it into the liquid chromatograph, record the chromatogram, and the results are shown in Table 7.

[0063] Table 7 linear experiment results

[0064]

[0065] It can be seen from Table 7 that within the range of 3.11-15.54 μg / ml, the detection method of the present invention has a good linear relationship.

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Abstract

The invention discloses a method for detecting a peramivir intermediate I by reversed-phase high performance liquid chromatography. The method comprises the following steps: preparing a test sample solution, detecting a test sample by reversed-phase high performance liquid chromatography, and calculating the contents of single impurities and total impurities in the test sample according to an area normalization method. According to the method, the intermediate I is completely separated from chromatographic peaks of various impurities by changing a mobile phase, a ratio, the wavelength of an ultraviolet absorption detector and the like; and the detection time is short, the detection specificity, accuracy and sensitivity are high, and more accurate detection and quality control can be carried out on the peramivir intermediate I.

Description

technical field [0001] The invention relates to a detection method of a peramivir intermediate, in particular to a reversed-phase high performance liquid chromatography detection method of a peramivir trihydrate intermediate I. Background technique [0002] The main intermediate I in the synthesis of peramivir is tert-butyl (3aR, 4R, 6R, 6aS)-6-(hydroxymethyl)-3-(pent-3-yl)-3a,5,6,6a-tetra Hydrogen-4H-cyclopentane[d]isoxazol-4-yl)carbamate with formula C 18 h 34 N 2 o 5 , the molecular weight is 358.5, and the structural formula is as follows, [0003] [0004] At present, there are many manufacturers supplying peramivir intermediates in the market, and the quality varies greatly. There are some impurity compounds. The existence of some impurities will seriously affect the quality and drug safety of peramivir, so it needs to be tested and quality controlled. . There are multiple pKas in the intermediate of peramivir, which makes it difficult to screen the pH of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/74
CPCG01N30/02G01N30/74Y02P20/55
Inventor 郭辉赵佳楠高文静李娜
Owner 日照正济药业有限公司
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