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Method for detecting related substances of retegravir intermediate

A detection method and technology for related substances, which are applied in the field of detection of related substances in intermediates of remdesivir, can solve the problems that there is no detection method for related substances in intermediates, and achieve the effects of stability, strong adaptability, and easy operation

Active Publication Date: 2021-04-30
JIANGSU LONG HEALTHCARE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no detection method for the related substances of the above-mentioned intermediates

Method used

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  • Method for detecting related substances of retegravir intermediate
  • Method for detecting related substances of retegravir intermediate
  • Method for detecting related substances of retegravir intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Embodiment 1: specificity test

[0040] 1. Detection of chromatographic conditions

[0041] Chromatographic column: C18 (250mm×4.6mm, 5μm);

[0042] Detector: Diode Array Detector (DAD);

[0043] Detection wavelength: 238nm;

[0044] Flow rate: 1.0ml / min;

[0045] Column temperature: 30°C;

[0046] Diluent: 0.1% phosphoric acid water-methanol (95:5);

[0047] Injection volume: 5 μl.

[0048] 2. Preparation of reference substance and test solution

[0049] The specificity test needs to verify that the blank solution has no interference at the retention time of the main peak in the test product and the reference solution, and the separation between impurities and main components.

[0050] The following is the preparation method of each impurity and main component:

[0051]Impurity a positioning solution: Accurately weigh 15 mg of impurity a reference substance, put in a 50 ml measuring bottle, add 5 ml of methanol first, then add 0.25 ml of 85% phosphoric acid, di...

Embodiment 2

[0067] Embodiment 2: sensitivity test

[0068] 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.

[0069] With reference to the detection chromatographic conditions of Example 1, accurately measure 5 μl of each of the above solutions, inject them into a liquid chromatograph, inject 6 injections of the quantification limit solution continuously, inject 1 injection of the detection limit solution, and record the chromatogram. The results are shown in Table 2~ table 3.

[0070] Table 2 Quantitative limit verification results

[0071] name Concentrationμg / ml S / N Sensitivity (%) Impurity a 0.11708 24.68 0.05 Impurity b 0.11746 38.48 0.05 intermediate 0.12240 21.07 0.05 ...

Embodiment 3

[0075] Embodiment 3: repeatability test

[0076] The test solution: Weigh about 12.5mg of the test product, put it in a 50ml measuring bottle, first add 5ml of methanol, then add 0.25ml of 85% phosphoric acid, dissolve it by ultrasonic, dilute with mobile phase A to the volume, shake well, Prepare 6 copies in parallel.

[0077] With reference to the detection chromatographic conditions of Example 1, 5 μl of each of the above solutions were precisely measured, injected into a liquid chromatograph, and the chromatogram was recorded. The results are shown in Table 4.

[0078] Table 4 Repeatability inspection results

[0079]

[0080]

[0081] Note: "ND" means not detected.

[0082] As can be seen from Table 4, the number of impurity peaks above the limit of quantification remains unchanged, and the RSDs of single impurity content and purity all meet the requirements (the RSD of each impurity with a content of less than 0.5% is not more than 10.0%; Each impurity RSD is no...

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Abstract

The invention discloses a method for detecting related substances of a retegravir intermediate, the retegravir intermediate has a structure shown as a formula I, and the detection method comprises the following steps: (1) preparing a reference substance and a test solution; (2) detection: adopting a high performance liquid chromatography method, wherein a mobile phase A is an acidic buffer solution with the concentration of 0.05%-0.5%, a mobile phase B is an organic solvent, the detection wavelength is 220 nm-240 nm, and the elution gradient mobile phase A comprises the following components in percentage by volume: 0 minute: 100%->90%, , 0-15minutes: 95%->50%, 15-30minutes: 50%-0%, and 30-50minutes: 100%->90%; and (3) calculating the content of related substances in the detection map in the step (2). According to the detection method, a specific detection method of the retegravir intermediate is established, the content of each related substance in the retegravir intermediate can be accurately detected, and the specificity, the sensitivity, the repeatability and the stability are good.

Description

technical field [0001] The present invention relates to a method for detecting related substances in a remdesivir intermediate, in particular to a method for detecting related substances in a remdesivir intermediate that can accurately detect the content of each related substance therein. Background technique [0002] Remdesivir (Remdesivir), developed by Gilead Sciences, is a nucleoside analog with antiviral activity. In HAE cells, the EC against SARS-CoV and MERS-CoV 50 The value is 74nM, in delayed brain tumor cells, EC against murine hepatitis virus 50 The value is 30 nM. Its chemical name is (S)-2-(((S)-(((2R,3S,4R,5R)-5-(4-aminopyrrolo[2,1-f][1,2,4] Triazin-7-yl)-5-cyano-3,4-dihydroxytetrahydrofuran-2-yl)methoxy)(phenoxy)phosphoryl)amino)propanoic acid-2-ethylbutyl ester, The English name is (S)-2-ethylbutyl-2-(((S)-(((2R,3S,4R,5R)-5-(4-aminopyrrolo-[2,1-f][1,2, 4]-triazin-7-yl)-5-cyano-3,4-dihydroxytetrahydrofuran-2-yl)methoxy)(phenoxy)phosphoryl)amino)propanoate,...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/64G01N30/86
CPCG01N30/02G01N30/06G01N30/64G01N30/8679
Inventor 马燕罗锋林
Owner JIANGSU LONG HEALTHCARE
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