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High performance liquid chromatography method for separating carfilzomib and isomers

A high-performance liquid chromatography and diastereomer technology, applied in the field of analysis and detection, can solve the problems of high separation and detection cost, expensive life, short chiral chromatographic column, etc., and achieve low separation and detection cost and excellent separation effect. Effect

Active Publication Date: 2019-03-01
湖南泰新医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Li Haixia et al. provided a HPLC method for simultaneous determination of 3 chiral isomers in carfilzomib (document: Li Haixia et al., a HPLC method for simultaneous determination of 3 chiral isomers in carfilzomib, Chinese Pharmacist 2016, Volume 19, No. 6), but this method must rely on expensive and short-lived chiral chromatographic columns, and the cost of separation and detection is relatively high

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  • High performance liquid chromatography method for separating carfilzomib and isomers
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Embodiment Construction

[0020] The substantive content of the present invention will be specifically introduced below in conjunction with the embodiments. Due to space reasons, the description of the experimental process cannot be done in great detail. All the parts not described in detail in the experiment are routine operations well known to those skilled in the art.

[0021] 1. Experimental materials

[0022] Shimadzu LC-20AT high performance liquid chromatograph (equipped with LC-20AT pump, SIL-20A autosampler and SPD-M20A diode array detector, Japan Shimadzu company).

[0023] Agilent ZORBAX Extend-C18 chromatographic column (4.6mm×250mm, 5μm) is a product of Agilent Company.

[0024] Standard products of carfilzomib, enantiomers, diastereomer I and diastereomer II were purchased or self-produced, with a purity of not less than 95%. The chiral reagent (2S,4S)-1-Boc-4-aminopyrrolidine-2-carboxylic acid methyl ester was purchased with a purity of not less than 95%.

[0025] Acetonitrile and tetr...

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Abstract

The invention discloses a high performance liquid chromatography method for separating carfilzomib and isomers. Chromatographic parameters are as follows: chromatographic column: Agilent ZORBAX Extend-C18 column (4.6mm*250mm, 5mum); mobile phase A Phase: water-acetonitrile-tetrahydrofuran solution in the volume ratio of 75:20:5, containing 20 mM (2S, 4S)-1-Boc-4-aminopyrrolidine-2-methyl formate;mobile phase B phase: acetonitrile; gradient elution procedure: 0-8 min, 0% B; 8-35 min, 0%-100% B; 35-40 min, 100%-0% B; flow rate: 1.0 mL / min; column temperature: 35 DEG C. According to the method,the carfilzomib, an enantiomer, a diastereoisomer I and a diastereoisomer II can be effectively separated by using the conventional C18 chromatographic column by adding a chiral reagent (2S, 4S)-1-Boc-4-aminopyrrolidine-2-methyl formate, the separation effect is excellent, and the separation and detection cost is low.

Description

technical field [0001] The invention belongs to the field of analysis and detection, and in particular relates to a high performance liquid chromatography method for separating carfilzomib and its isomers. Background technique [0002] Carfilzomib (carfilzomib) is a second-generation proteasome inhibitor administered intravenously and has good antitumor activity. Immunomodulatory drugs), and there is evidence that the refractory multiple myeloma with disease progression within 60 days after the completion of the last treatment was approved by the FDA on July 20, 2012. [0003] During the production of carfilzomib, there may be enantiomers, diastereoisomer I and diastereoisomer II impurities (see the literature for the chemical structure: Li Haixia et al., an HPLC method for the simultaneous determination of carfilzomib The content of three chiral isomers in rice, Chinese Pharmacist, Volume 19, Issue 6, 2016), according to the requirements of impurity research, these isomer ...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 刘华平李月群金荣
Owner 湖南泰新医药科技有限公司