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Method for separating and determining methyhaaltrexone bromide and impurities thereof with liquid chromatography

A technology of methylnaltrexone bromide and liquid chromatography, which is applied in the direction of material separation, measuring devices, and analysis materials, can solve problems such as the inability to separate methylnaltrexone bromide, and achieve low cost, easy preparation, and accurate determination of impurities Effect

Active Publication Date: 2012-07-11
CHONGQING PHARMA RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Because the existing methods can not effectively separate bromidenaltrexone and its "S-N isomer", monohydroquinone and other impurities, in order to accurately control the quality of bromethylnaltrexone and monitor impurities, it is necessary to find a kind of energy Simple, rapid, accurate and effective method for separation and detection of bromethylnaltrexone and its related impurities

Method used

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  • Method for separating and determining methyhaaltrexone bromide and impurities thereof with liquid chromatography
  • Method for separating and determining methyhaaltrexone bromide and impurities thereof with liquid chromatography
  • Method for separating and determining methyhaaltrexone bromide and impurities thereof with liquid chromatography

Examples

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Effect test

Embodiment 1

[0046] Instruments and Conditions

[0047] Dianne Ultimate 3000 high-performance liquid chromatography and chemical workstation; automatic sample injection; with Breeze AQ-C18 (4.6 × 250mm, 5μm) as the chromatographic column; set the wavelength of the ultraviolet detector to 310nm; mobile phase: 0.1% trifluoroacetic acid Solution is mobile phase A, with methanol as mobile phase B, carry out gradient elution in the following manner:: 0 minute to 10 minutes, mobile phase A is 85% (V / V), mobile phase B is 15% (V / V V); 10 minutes to 35 minutes, mobile phase A linearly decreased to 60% (V / V), and mobile phase B linearly increased to 40% (V / V); 35 minutes to 45 minutes, mobile phase A was 60% ( V / V), mobile phase B is 40% (V / V); 45.1 minutes to 55 minutes, mobile phase A is 85% (V / V), mobile phase B is 15% (V / V), that is, 45.1 minutes followed by the equilibrated column. The column temperature was 30° C., the flow rate was 1.0 ml / min, and the injection volume was 20 μl.

[0048] ...

Embodiment 2

[0056] Determination of impurities in methylnaltrexone bromide injection by liquid chromatography.

[0057] Instruments and Conditions

[0058] Agilent 1200 high-performance liquid chromatography and chemical workstation; automatic sampling; chromatographic conditions are the same as in Example 1.

[0059] Take an appropriate amount of methylnaltrexone bromide injection (approximately equivalent to 10 mg of methylnaltrexone bromide), put it in a 10ml measuring bottle, add diluent (mobile phase A: mobile phase B=85:15) to dissolve and dilute to the mark, Shake up, as need testing solution; Precision measures 1.0ml, puts in 10ml measuring bottle, adds diluent and dilutes to scale, shakes up, as contrast solution; Carry out liquid chromatography analysis according to the chromatographic condition of embodiment 2, the results see Figure 5 , Image 6 . Figure 5 , Image 6 It shows that there is almost no impurity detected in the methylnaltrexone bromide bulk drug, indicating ...

Embodiment 3

[0061] Determination of Impurities in Brommethylnaltrexone APIs by Liquid Chromatography

[0062] Instruments and Conditions

[0063] Agilent 1200 high-performance liquid chromatography and chemical workstation; automatic sampling; chromatographic conditions are the same as in Example 1.

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Abstract

The invention provides a method for separating and determining methyhaaltrexone bromide and impurities and contents thereof with liquid chromatography. The method comprises the following steps: (a) adopting a chromatographic column using alkyl-silicane bonded silica gels as packing to be a separation column; (b) using a trifluoroacetic acid buffer solution as a flowing phase A, and using an organic solvent as a flowing phase B; and (c) and adopting gradient elution for the flowing phases, and separating and determining the impurities and contents of methyhaaltrexone bromide and a preparation thereof. According to the method, methyhaaltrexone and other known intermediate impurities as well as unknown impurities can be effectively separated and determined. The method has strong specificity, high accuracy and convenience for operation.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and be specifically related to the method for the separation and determination of methylnaltrexone bromide and its impurities by liquid chromatography (HPLC), the method comprising a using an alkylsilane-bonded silica gel as a chromatographic column for packing as a separation column: b The buffer solution is used as the mobile phase A, and the organic solvent is used as the mobile phase B; c The mobile phase adopts a gradient elution method. The method can effectively separate and determine bromidenaltrexone and its related substances. Background technique [0002] Methylnaltrexone bromide is a peripheral opioid receptor antagonist with the molecular formula C 21 h 26 o 4 NBr, its structural formula sees below (I). The chemical name of methylnaltrexone bromide is: 17-(cyclopropylmethyl)-4,5α-epoxy-3,14-dihydroxy-17-methyl-6-oxo-morphinan bromide, which has a Nitrogen chiral center. The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/60G01N30/34G01N30/06
Inventor 廖薇张道林付晓泰刘泽荣孙化富樊斌
Owner CHONGQING PHARMA RES INST
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