Method for determining content of methanesulfonic acid in busulfan

A determination method and technology of methanesulfonic acid, applied in the field of medicine, can solve the problems such as the method without the content of methanesulfonic acid in busulfan

Inactive Publication Date: 2018-12-11
SHANGHAI AOBO PHARMTECH INC LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, in the Pharmacopoeia, busulfan adopts titration method to measure total acidity, and there is no exclusive method for measuring the content of methanesulfonic acid in busulfan. The present invention adopts high performance liquid chromatography and CAD to measure the content of methanesulfonic acid in busulfan

Method used

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  • Method for determining content of methanesulfonic acid in busulfan
  • Method for determining content of methanesulfonic acid in busulfan
  • Method for determining content of methanesulfonic acid in busulfan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Instruments and Conditions:

[0029] HPLC equipped with CAD: Ultimate 3000, DIONEX Corona Veo RS CAD

[0030] Chromatographic column: ion chromatography column

[0031] Mobile phase: A: 0.1% trifluoroacetic acid in water B: 0.2% trifluoroacetic acid in acetonitrile.

[0032] The gradient is as follows: 0min-20min, the proportion of organic phase is 5%-95%; 20min-20.1min, the proportion of organic phase is 95%-5%; 20.1min-30min, the proportion of organic phase is 5%.

[0033] Flow rate: 1.0mL / min

[0034] Column temperature: 25°C

[0035] Vaporization temperature: 25°C

[0036] Injection volume: 5μL

[0037] Collection time: 21min

[0038] Diluent: Acetonitrile

[0039] Experimental steps:

[0040] Blank sample: pipette 1.0mL of acetonitrile into a 2mL HPLC vial and inject. Record the chromatogram, typical spectrum see figure 1 .

Embodiment 2

[0042] Instruments and Conditions:

[0043] HPLC equipped with CAD: Ultimate 3000, DIONEX Corona Veo RS CAD

[0044] Chromatographic column: ion chromatography column

[0045] Mobile phase: A: 0.1% trifluoroacetic acid in water B: 0.2% trifluoroacetic acid in acetonitrile.

[0046] The gradient is as follows: 0min-20min, the proportion of organic phase is 5%-95%; 20min-20.1min, the proportion of organic phase is 95%-5%; 20.1min-30min, the proportion of organic phase is 5%.

[0047] Column temperature: 25°C

[0048] Vaporization temperature: 25°C

[0049] Injection volume: 5μL

[0050] Collection time: 21min

[0051] Diluent: Acetonitrile

[0052] Experimental steps:

[0053] (1) Brenitrazam and methanesulfonic acid stock solution A: Weigh 50 mg of the white nitramide reference substance and 50 mg of the methanesulfonic acid reference substance, accurately weigh it in a 25 mL volumetric flask, dissolve it with diluent and dilute to the mark, and mix well. (Dinitrazol co...

Embodiment 3

[0056] Instruments and Conditions:

[0057] HPLC equipped with CAD detectors: Ultimate 3000, DIONEX Corona Veo RS CAD

[0058] Chromatographic column: ion chromatography column

[0059] Mobile phase: A: 0.1% trifluoroacetic acid in water B: 0.2% trifluoroacetic acid in acetonitrile.

[0060] The gradient is as follows: 0min-20min, the proportion of organic phase is 5%-95%; 20min-20.1min, the proportion of organic phase is 95%-5%; 20.1min-30min, the proportion of organic phase is 5%.

[0061] Flow rate: 1.0mL / min

[0062] Column temperature: 25°C

[0063] Vaporization temperature: 25°C

[0064] Injection volume: 5μL

[0065] Collection time: 21min

[0066] Diluent: Acetonitrile

[0067] Experimental steps:

[0068] (1) Brenitrazam and methanesulfonic acid stock solution A: Weigh 50 mg of the white nitramide reference substance and 50 mg of the methanesulfonic acid reference substance, accurately weigh it in a 25 mL volumetric flask, dissolve it with diluent and dilute t...

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Abstract

The invention discloses a method for determining the content of methanesulfonic acid in busulfan. According to the method, the content of methanesulfonic acid is directly determined through the combination of a high performance liquid chromatography and a charged aerosol detector (hereinafter CAD for short). Compared with the prior art, the analysis method has the characteristics of simplicity inreproducibility, good in specificity, high in sensitivity and the like.

Description

technical field [0001] The present invention relates to directly measuring the content of methanesulfonic acid by combining high performance liquid chromatography and electric aerosol detector (hereinafter referred to as: CAD), so as to calculate the content of methanesulfonic acid in busulfan. The method can better control the content of methanesulfonic acid in the crude drug and provide guarantee for patients' healthy drug use, and belongs to the technical field of medicine. technical background [0002] Busulfan, whose chemical name is 1,4-butanediol dimesylate, is mainly used in the treatment of chronic myelogenous leukemia, polycythemia vera, and myelofibrosis. The structural formula of Busulfan is as follows: [0003] [0004] Methanesulfonyl chloride is used as raw material in the synthesis process of Busulfan crude drug, and methylsulfonyl chloride is hydrolyzed to form methanesulfonic acid, and the structure of methanesulfonic acid is as follows: [0005] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 尹巧珍邱学艳胡素招安建国黄鲁宁陈茜顾虹
Owner SHANGHAI AOBO PHARMTECH INC LTD
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