Method for separating and measuring Palonosetron hydrochloride and optical isomers thereof

A technology of optical isomers and palonosetron, applied in the field of separation and determination of palonosetron hydrochloride and its optical isomers, can solve the problems of chromatographic peaks that cannot be separated, separated, separated, etc.

Active Publication Date: 2010-03-03
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the chromatographic method using a commonly used packing chromatographic column cannot separate palonosetron hydrochloride from the isomer (3aS, S), because the chromatographic peaks completely overlap and cannot be separated; the commonly used packing chromatographic column cannot be separated between other isomers , such as isomers (3aS, R) and (3aR, S) chromatographic peaks also completely overlap and cannot be separated
It is even more impossible to determine the content of several isomers separately

Method used

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  • Method for separating and measuring Palonosetron hydrochloride and optical isomers thereof
  • Method for separating and measuring Palonosetron hydrochloride and optical isomers thereof
  • Method for separating and measuring Palonosetron hydrochloride and optical isomers thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Chromatography, mass spectrometry and detection limit basic research of four kinds of optical isomers of embodiment 1

[0027] Experimental equipment and conditions

[0028] a, HPLC (high performance liquid chromatography) conditions

[0029] Instrument: SHIMADZU LC-2010A HT (Shimadzu, Japan)

[0030] Detector: UV

[0031] Mobile phase: 0.3% triethylamine (adjust pH4.0 with glacial acetic acid)-methanol (30:70)

[0032] Chromatographic column: CHIROBIOTIC T 4.6×250mm 5μm

[0033] Flow rate: 1.0ml / min

[0034] Detection wavelength: 249nm

[0035] Chromatography Workstation: LCsolution

[0036] b. MS (mass spectrometry) conditions

[0037] MS instrument: API3000 (American Bio-Application Engineering Company)

[0038] Ion Source: Turbo Spray

[0039] Ion Source Gas1 (GS1): 4.0

[0040] Curtain gas: 10.0

[0041] Ion Source Gas2 (GS2): 0.0

[0042] DP: 60.0

[0043] EP: 12.0

[0044] IS: 5500.00

[0045] method study

[0046] a. LC qualitative

[0047] Tak...

Embodiment 2

[0061] Determination of other optical isomers content in the Palonosetron hydrochloride bulk drug in embodiment 2

[0062] a, Determination method

[0063] Use macrocyclic glycopeptide Teicoplanin (Teicoplanin) bonded silica gel as filler (CHIROBIOTIC T 4.6×250mm5μm); use 0.3% triethylamine (adjust pH4.0 with glacial acetic acid)-methanol (30:70) as mobile phase ; The detection wavelength is 249nm. Take an appropriate amount of (3aS, S), (3aR, S), (3aS, R), (3aR, R) mixtures, add mobile phase to dissolve and dilute to a solution of about 0.2mg per 1ml, and inject samples according to the above chromatographic conditions 20 μl, record the chromatogram. According to the order of peaks, peak 1 is (3aS, S), peak 2 is (3aR, S), peak 3 and peak 4 are (3aS, R), two components of (3aR, R) mixture. The number of theoretical plates calculated by (3aS, S) should not be less than 4000, and the separation degree of palonosetron hydrochloride peaks and adjacent isomers should not be less...

Embodiment 3

[0071] Other optical isomer content determination in embodiment 3 Palonosetron hydrochloride injection

[0072] a, Determination method

[0073] Use macrocyclic glycopeptide Teicoplanin (Teicoplanin) bonded silica gel as filler (CHIROBIOTIC T4.6×250mm5μm); use 0.3% triethylamine (adjust pH4.0 with glacial acetic acid)-methanol (30:70) as flow phase; the detection wavelength is 249nm. Take an appropriate amount of (3aS, S), (3aR, S), (3aS, R), (3aR, R) mixtures, add mobile phase to dissolve and dilute to a solution of about 0.2mg per 1ml, and inject samples according to the above chromatographic conditions 20 μl, record the chromatogram. According to the order of peaks, peak 1 is (3aS, S), peak 2 is (3aR, S), peak 3 and peak 4 are (3aS, R), two components of (3aR, R) mixture. The number of theoretical plates calculated by (3aS, S) should not be less than 4000, and the separation degree of palonosetron hydrochloride peaks and adjacent isomers should not be less than 1.0

[0...

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Abstract

The invention relates to a method for separating and measuring content of Palonosetron hydrochloride and optical isomers thereof by high performance liquid chromatography, which is characterized in that: a chromatographic column packing material used in the high performance liquid chromatography is macrocyclic glycopeptides and teicoplanin bonded silica gel, and a mobile phase consists of aqueoussolution of triethylamine and organic solvent.

Description

Technical field: [0001] The invention relates to a method for separating and measuring palonosetron hydrochloride and its optical isomers, in particular to separating palonosetron hydrochloride and its other three optical isomers by high performance liquid chromatography and methods of content determination. Background technique: [0002] Palonosetron hydrochloride (chemical name (3aS)-2-[(S)-1-azabicyclo[2.2.2]oct-3-yl]-2,3,3a,4,5,6-hexa Hydrogen-1-oxo-1H-benzo[de]isoquinoline hydrochloride) is a drug that has a stronger binding force to 5-HT3 receptors and is clinically used to prevent Acute and delayed emesis caused by emetic chemotherapy regimens. [0003] Since palonosetron hydrochloride contains two chiral centers, in addition to (3aS, S type) palonosetron hydrochloride, there are three other optical isomers: (3aR, S), (3aS, R) , (3aR, R), and these three isomers have no above-mentioned drug activity. Therefore, the separation of palonosetron hydrochloride from the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02B01D15/00
Inventor 杨平
Owner CHONGQING HUAPONT PHARMA
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