Method for simultaneously determining four optical isomers of palonosetron hydrochloride

A technology of optical isomers and palonosetron, which is applied in the fields of organic chemistry, chemical instruments and methods, organic chemistry, etc., can solve the analytical method that has not yet been reported to achieve chromatographic separation at one time, does not achieve one-time separation, and is cumbersome. And other issues

Active Publication Date: 2011-10-05
SHENZHEN NEPTUNUS PHARM CO LTD
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  • Claims
  • Application Information

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Problems solved by technology

Bai Jiangtao disclosed a method for separating four isomers in the Chinese patent application [Application No. 200710074410.0], which has made great progress. However, in the actual test operation, this method is to adjust the temperature twice, that is, to inject Twice, and the separation is relatively complicated and cumbersome, and each time the chromatographi

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  • Method for simultaneously determining four optical isomers of palonosetron hydrochloride
  • Method for simultaneously determining four optical isomers of palonosetron hydrochloride
  • Method for simultaneously determining four optical isomers of palonosetron hydrochloride

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Embodiment

[0017] Embodiment, simultaneous determination of four optical isomers of palonosetron hydrochloride

[0018] 1. Instruments and reagents

[0019] 1.1 Instruments and reagents

[0020] Instrument: Agilent 1100series high performance liquid chromatography, chromatographic grade acetonitrile, isopropanol (Merck), diethylamine (analytical grade).

[0021] Reagents: S.R, R.S, R.R type isomers (self-made or purchased from the market), palonosetron hydrochloride raw materials (provided by Shenzhen Neptune Pharmaceutical Co., Ltd., batch numbers 20080601, 20080602, 20080603).

[0022] 1.2 Chromatographic conditions:

[0023] Chromatographic column: CHIRALPAK OD-H 5μm 4.6×250mm chiral chromatographic column (manufactured by DAICEL)

[0024] Mobile phase: acetonitrile: isopropanol: diethylamine (the volume ratio of the three is 82-92: 18-8: 0.1-0.2; and preferably 85: 15: 0.1)

[0025] Flow rate: 0.3-1.2ml / min (preferably 1.0ml / min), injection volume: 5μl.

[0026] Column temperatu...

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Abstract

The invention discloses a method for simultaneously determining four optical isomers of palonosetron hydrochloride. The four optical isomers are S.S, S.R, R.S, R.R respectively; and the method is characterized by comprising the following step of splitting the optical isomers of the palonosetron hydrochloride by using efficient liquid chromatography, wherein an OD-H chiral chromatographic column is included, and a mobile phase consists of acetonitrile, isopropanol and diethylamine in a volume ratio of (82-92): (18-8): (0.1-0.2), and the column temperature is 30 to 40 DEG C. A flow rate in the efficient liquid chromatography is 0.3 to 1.2 ml/min. The detection wavelength in the efficient liquid chromatography is 220nm. The method is simple, convenient and practical. The purpose of simultaneously determining and separating the four optical isomers can be rapidly achieved, a basis is provided for quality control of palonosetron hydrochloride raw materials and preparations, and the quality control of a new medicine is facilitated.

Description

technical field [0001] The invention relates to a method for separating and measuring optical isomers of palonosetron hydrochloride, in particular to a method for simultaneously measuring four optical isomers of palonosetron hydrochloride. Background technique [0002] Palonosetron hydrochloride (Palonosetron) is a highly selective 5-HT receptor antagonist (see the figure below for the structural formula, C 19 h 24 N 2 O·HCL), which can block the excitation of presynaptic 5-HT receptors in the peripheral neurons of the vomiting reflex center, and reduce the incidence of vomiting and nausea. The drug is currently in clinical use. [0003] The structural formula is: [0004] [0005] Palonosetron hydrochloride exerts its pharmacological effects in the SS configuration, and its isomers RR, RS, and SR have no biological effects. In the preparation process and sample preservation, it is very important to monitor its isomers, so as to understand the interference with the ma...

Claims

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Application Information

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IPC IPC(8): G01N30/06C07D453/02C07B57/00
Inventor 李勇陈萍李姿高媛唐田严启新
Owner SHENZHEN NEPTUNUS PHARM CO LTD
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