A kind of detection method of related substance in rifampicin

A detection method and a technology for related substances, which are applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems that there are no relevant literature reports on the detection methods of N-methylpiperazine and 1-amino-4-methylpiperazine, etc. Achieve the effect suitable for practical application and promotion, good linear relationship and high precision

Active Publication Date: 2022-03-25
HEBEI XINGANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] By-products or unreacted raw materials, such as N-methylpiperazine and 1-amino-4-methylpiperazine, may be introduced in the process of synthesizing rifampicin raw materials in the existing process, and there is no relevant literature report at present Detection method of N-methylpiperazine and 1-amino-4-methylpiperazine

Method used

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  • A kind of detection method of related substance in rifampicin
  • A kind of detection method of related substance in rifampicin
  • A kind of detection method of related substance in rifampicin

Examples

Experimental program
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Effect test

Embodiment 1

[0045] The embodiment of the present application provides a method for detecting a related substance in rifampicin, and the method for detecting comprises the following steps:

[0046] Step 1. Prepare blank solution, test solution, reference solution and 100% test solution fortification:

[0047] The blank solution is acetonitrile solvent;

[0048] Preparation of the test solution: take 50mg of rifampicin sample, accurately weigh it, place it in a 5mL volumetric flask, add acetonitrile to dissolve and dilute to the mark, shake well, and use it as the test solution;

[0049] Preparation of reference substance stock solution: respectively take 62 mg of N-methylpiperazine reference substance and 1-amino-4-methylpiperazine reference substance, accurately weigh them, put them in a 50mL volumetric flask, add acetonitrile to dissolve and dilute to the mark , shake well; then transfer 1.0mL of the above solution to a 50mL volumetric flask, add acetonitrile to dilute to the mark, shak...

Embodiment 2

[0060] Example 2 Repeatability

[0061] The repeatability of N-methylpiperazine: take the same batch of samples, prepare 6 parts of 100% test sample spiked solutions in parallel, and use liquid chromatography-mass spectrometry to detect. The specific conditions of liquid chromatography and mass spectrometry are as described in Example 1, and the results are shown in Table 1.

[0062] Wherein, the preparation method of the above-mentioned 100% test substance spiked solution is: take about 50 mg of rifampicin sample, accurately weigh it, place it in a 5mL volumetric flask, accurately add 2.0mL reference substance stock solution, and then add acetonitrile to make the volume up to the mark , Shake well, as 100% test sample spiked solution.

[0063] The repeatability of 1-amino-4-methylpiperazine: take the same batch of samples, prepare 6 parts of 100% spiked solution of the test product in parallel, and use liquid chromatography-mass spectrometry for detection. The specific chara...

Embodiment 3

[0068] Example 3 intermediate precision

[0069] Intermediate precision solution: take the same batch of samples, prepare 6 parts of 100% standard spiked solution in parallel, and use different instruments in the same laboratory at different times for liquid chromatography-mass spectrometry detection. The conditions are as described in Example 1, and the results are shown in Table 2.

[0070] The preparation method of above-mentioned 100% need testing product standard addition solution is: get about 40mg of rifampicin sample, weigh accurately, place 5mL volumetric flask, accurately add 2.0mL reference substance stock solution, then add acetonitrile to be settled to scale, shake Uniformly, as 100% test sample spiked solution.

[0071] Table 2 Intermediate precision results

[0072]

[0073] It can be seen from Table 2 that the RSD of the content of each analyte in the 6 intermediate precision solutions is less than or equal to 10.0%, indicating that the intermediate precis...

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Abstract

The invention relates to the technical field of drug analysis, and specifically discloses a method for detecting related substances in rifampicin. The method comprises: preparing a test solution and a reference solution, and detecting by liquid chromatography-mass spectrometry, wherein the liquid chromatography adopts a C18 chromatographic column, and a formic acid aqueous solution with a volume concentration of 0.8‰~1.2‰ is used as a flow Phase A, using acetonitrile as mobile phase B, gradient elution; the mass spectrometer adopts ESI ion source, positive ion detection, SIM mode. The detection method provided by this application has the advantages of simple method, stability, high precision, good reproducibility, etc., and can quickly and accurately detect the impurities N-methylpiperazine and 1-amino-4- The whole operation process is reliable and controllable, suitable for practical application and promotion, and has broad application prospects.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for detecting related substances in rifampicin. Background technique [0002] Rifampicin, molecular formula C 43 H 58 N 4 O 12 , invented in 1965, is a rifamycin semi-synthetic broad-spectrum antibiotic, an important anti-tuberculosis drug. The discovery of rifampicin has made a bigger leap in the treatment of tuberculosis. In addition to its high activity against Mycobacterium tuberculosis, it has high activity against Staphylococcus aureus, non-enterococcal streptococci and monocytogenes lys. Tertella is also highly active; it is also the most effective treatment for non-pulmonary tuberculosis including tuberculous meningitis. [0003] By-products or unreacted raw materials, such as N-methylpiperazine and 1-amino-4-methylpiperazine, may be introduced in the process of synthesizing rifampicin bulk drugs in the existing process, and there is no relevant litera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/72G01N30/8637G01N2030/324
Inventor 李海东史守坤章万志康翠雪王香英刘爱军
Owner HEBEI XINGANG PHARMA
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