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High-performance liquid chromatography for separating linezolide and chiral isomer thereof

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

Active Publication Date: 2019-03-08
SUZHOU LEO BIOTECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The literature provides a method for separating linezolid and its isomer (R)-linezolid (document: Liu Xiao et al., chiral HPLC analysis of R-type isomer in linezolid raw material drug, foreign pharmaceutical antibiotics Volume 37, No. 4, July 2016), but this method must rely on expensive and short-lived chiral chromatographic columns, and the cost is high

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  • High-performance liquid chromatography for separating linezolide and chiral isomer thereof
  • High-performance liquid chromatography for separating linezolide and chiral isomer thereof
  • High-performance liquid chromatography for separating linezolide and chiral isomer thereof

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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] Standards of linezolid and (R)-linezolid were purchased or self-made, with a purity of not less than 95%.

[0025] The chiral reagent (3S,4R)-1-Cbz-4-methylpyrrolidine-3-carboxylic acid was purchased with a purity of not less than 95%.

[0026] Acetonitrile and pyridine are chromatographically pure, and water is ...

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Abstract

The invention discloses ahigh-performance liquid chromatography for separating linezolide and a chiral isomer thereof. Chromatographic parameters are as follows: a chromatographic column: Agilent ZORBAX Extend-C18 chromatographic column (4.6mm*250mm, 5mum); a moving phase A phase: a water-acetonitrile-pyridine solution with a volume ratio of 82:10:8, wherein 20 mM of (3S, 4R)-1-Cbz-4-methylpyrrolidine-3-carboxylic acid; a moving phase B phase: acetonitrile; a gradient elution program: 0-7 min, 0% B; 7-30 min, 0%-90% B; 30-40 min, 90%-0% B; a flow speed: 1.0 mL / min; and a column temperature: 35DEG C. According to the invention, a chiral reagent (3S, 4R)-1-Cbz-4-methylpyrrolidine-3-carboxylic acid is added, so that the linezolide and the chiral isomer thereof can be effectively separated byusing the conventional C18 chromatographic column; the separating effect is excellent; andthe separating and detecting cost is low.

Description

technical field [0001] The invention belongs to the field of analysis and detection, and relates to a high performance liquid chromatography method for separating linezolid and its chiral isomer. Background technique [0002] Linezolid chemical name: (S)-5-(acetamidomethyl)-3-[(3-fluoro-4-morpholinyl)phenyl]-1,3-oxazolidine-2 - Ketone, trade name: Zyvox, is a new type of oxazolidinone antibacterial drug developed by Pharmacia & Upjohn Company, which was first listed in the United States in April 2000. It is clinically used to treat infections caused by Gram-positive cocci, including suspected or confirmed nosocomial-acquired pneumonia (HAP), community-acquired pneumonia (CAP), complicated skin or skin and soft tissue infection (SSTI) caused by MRSA, and vancomycin-resistant Veterinary Enterococcus (VRE) infection. There is a chiral center in the molecular structure of linezolid, and there is a pair of optical isomers (structural formula is as follows), the pharmacologicall...

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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 SUZHOU LEO BIOTECH