A detection method for related substances of remdesivir 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: 2022-05-27
JIANGSU LONG HEALTHCARE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A detection method for related substances of remdesivir intermediate
  • A detection method for related substances of remdesivir intermediate
  • A detection method for related substances of remdesivir intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 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℃;

[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 solution and the reference solution, as well as the resolution between the impurities and the main components.

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

[0051]Impurity a positioning solution: Precisely weigh 15 mg of the impurity a reference substance, put it in a 50 ml volumetric flask, add 5 ml of methanol, add 0.25 ml of 85% phosphoric a...

Embodiment 2

[0067] Example 2: Sensitivity test

[0068] Take the system suitability solution prepared in Example 1, dilute it to appropriate multiples step by step, take the solution with signal-to-noise ratio ≥ 10:1 as the limit of quantitation solution; take the solution with signal-to-noise ratio ≥ 3:1 as the limit of detection solution.

[0069] Referring to the detection chromatographic conditions of Example 1, 5 μl of each of the above solutions were accurately measured and injected into a liquid chromatograph, 6 injections of the limit of quantification solution and 1 injection of the detection limit solution were performed continuously, and the chromatogram was recorded. The results are shown in Table 2~ table 3.

[0070] Table 2 Validation results of the limit of quantification

[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 Impurity c 0....

Embodiment 3

[0075] Example 3: Repeatability test

[0076] Test solution: Weigh about 12.5mg of the test product, put it in a 50ml volumetric flask, first add 5ml of methanol, then add 0.25ml of 85% phosphoric acid, ultrasonically dissolve it, dilute it with mobile phase A to the mark, shake well, 6 servings were prepared in parallel.

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

[0078] Table 4 Repeatability investigation results

[0079]

[0080]

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

[0082] It can be seen from Table 4 that the number of impurity peaks above the quantitative limit remains unchanged, and the RSD of single impurity content and purity meet the requirements (the RSD of each impurity with a content of less than 0.5% is not greater than 10.0%; The RSD of each imp...

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Abstract

The invention discloses a method for detecting related substances of a remdesivir intermediate. The remdesivir intermediate has a structure of formula I. The detection method comprises the following steps: (1) preparing a reference substance and a test solution (2) Detection: adopt high performance liquid chromatography, mobile phase A is 0.05%~0.5% acidic buffer, mobile phase B is organic solvent, detection wavelength is 220nm~240nm, elution gradient mobile phase A is with volume ratio Calculated, 0 minutes: 100%→90%, 0~15 minutes: 95%→50%, 15~30 minutes: 50%→0%, 30~50 minutes: 100%→90%; (3) Calculation steps ( 2) The content of related substances in the detection spectrum. This detection method has established a unique detection method for the intermediate of remdesivir, which can accurately detect the content of various related substances in it, and has good specificity, sensitivity, repeatability and stability.

Description

technical field [0001] The invention relates to a detection method for a related substance of a remdesivir intermediate, in particular to a detection method for a related substance of a remdesivir intermediate that can accurately detect the content of each related substance therein. Background technique [0002] Remdesivir, developed by Gilead Sciences, is a nucleoside analog with antiviral activity against EC of SARS-CoV and MERS-CoV in HAE cells 50 Value of 74 nM, EC against murine hepatitis virus in delayed brain tumor cells 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)propionic acid-2-ethylbutyl ester, English name (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, its CAS number is: 1809249-37-3...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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