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Method for analyzing benserazide impurity A in levodopa and benserazide hydrochloride compound preparation

A compound preparation and dopasehydrazine technology, applied in the field of drug analysis and detection, can solve the problems of low accuracy, low sensitivity at low concentration, unsatisfactory recovery rate and the like

Pending Publication Date: 2020-10-23
ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the existing HPLC methods for detecting benserazide impurity A in dopasrazide compound preparations use common liquid chromatography columns such as C18. These methods have low sensitivity at low concentrations, small response, and large interference from excipients, resulting in low accuracy , the recovery rate did not meet the requirements, and in the subsequent sample testing process, it was found that the content of benserazide impurity A was low, which caused quality problems

Method used

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  • Method for analyzing benserazide impurity A in levodopa and benserazide hydrochloride compound preparation
  • Method for analyzing benserazide impurity A in levodopa and benserazide hydrochloride compound preparation
  • Method for analyzing benserazide impurity A in levodopa and benserazide hydrochloride compound preparation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Chromatographic conditions:

[0076] Instrument: High performance liquid chromatography equipped with UV detector

[0077] Chromatographic column: Ultimate AQ C18 4.6*250mm 5μm (filler: B-type ultra-high purity fully porous spherical silica gel filler)

[0078] Mobile phase A: Add 2.2g sodium heptanesulfonate + 6.8g potassium dihydrogen phosphate to 1L water, adjust pH to 6.0 with 5M sodium hydroxide

[0079] Mobile Phase B: Methanol

[0080] Detection wavelength: 210nm

[0081] Flow rate: 1.0mL / min

[0082] Injection volume: 10μL

[0083] Column temperature: 30°C

[0084] Sample chamber temperature: 4°C

[0085] Running time: 60min

[0086] time / min Mobile phase A / % Mobile phase B / % 0-15 100 0 15-35 100→30 0→70

[0087] Diluent: 70% Methanol

[0088] Blank solution preparation:

[0089] with diluent.

[0090] Linear solution 1:

[0091] Weigh an appropriate amount of benserazide impurity A reference substance, dilute with a dil...

Embodiment 2

[0109] Chromatographic conditions: change the pH in the mobile phase A, adjust the pH to 7.0 with 5M sodium hydroxide, and keep other conditions unchanged.

[0110] Diluent: 70% Methanol

[0111] Resolution solution (system suitability solution):

[0112] Get the separation degree solution of embodiment 1 and carry out detection and analysis by above-mentioned detection condition, system suitability chromatogram is shown in Figure 8 . Figure 8 The peak order of each component in the product is levodopa, benserazide impurity A, levodopa impurity B, the peak elution time is 5.988min, 4.686min, 8.195min, and their resolutions are 2.78, 3.88, All chromatographic parameters meet the requirements.

[0113] Accuracy (0.1%) solution:

[0114] Weigh 1000mg of levodopa and 1698mg of blank excipients into a 100ml measuring bottle, accurately measure 1ml of benserazide impurity A accuracy stock solution into the same measuring bottle, add diluent to 2 / 3 volume of the measuring bottl...

Embodiment 3

[0117] Chromatographic conditions: change the pH in the mobile phase A, adjust the pH to 2.0 with phosphoric acid, and keep other conditions unchanged.

[0118] Diluent: 70% Methanol

[0119] Resolution solution (system suitability solution):

[0120] Get the separation degree solution of embodiment 1 and carry out detection and analysis by above-mentioned detection condition, system suitability chromatogram is shown in Figure 10 . Figure 10 The order of the peaks of each component in the product is levodopa, benserazide impurity A, levodopa impurity B, the peak elution time is 29.710min, 30.141min, 30.722min, and their resolutions are 2.35, 3.38, All chromatographic parameters meet the requirements.

[0121] Accuracy (0.1%) solution:

[0122] Weigh 1000mg of levodopa and 1698mg of blank excipients into a 100ml measuring bottle, accurately measure 1ml of benserazide impurity A accuracy stock solution into the same measuring bottle, add diluent to 2 / 3 volume of the measur...

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Abstract

The invention provides a method for detecting the content of a benserazide impurity A in a levodopa and benserazide hydrochloride compound preparation. According to the method, a hydrophilic chromatographic column is adopted, an aqueous solution containing sodium heptanesulfonate and monopotassium phosphate and having a pH value of 1.7-9.0 is adopted as a mobile phase A, methanol is adopted as a mobile phase B, and a staged gradient elution method is adopted to separate a benserazide impurity A and determine the content of the benserazide impurity A in a levodopa and benserazide hydrochloridecompound preparation. The method is good in separation effect, simple to operate, high in recovery rate, high in sensitivity and wide in linear range, and has important practical significance in the aspect of quality control in the preparation process of the preparation.

Description

technical field [0001] The invention belongs to the field of drug analysis and detection, and in particular relates to an HPLC method for detecting the benserazide impurity A(2RS)-2-amino-3-hydroxypropionylhydrazide in a compound preparation of dopasrazide. Background technique [0002] The dopaserazide compound tablet prepared by the original research company Roche Holding AG, whose trade name is Madopar (Madopa), consists of levodopa and benserazide hydrochloride, and is used for the treatment of Parkinson's or Parkinson's syndrome (post-encephalitis, Arteriosclerotic or toxic) drugs. This drug can increase the content of dopamine in brain cells and improve Parkinson's symptoms. At the same time, benserazide can prevent dopa decarboxylase from being converted into dopamine before levodopa enters the brain, thereby increasing dopamine in the brain, enhancing its curative effect and reducing its peripheral adverse reactions. As the first-line drug for the treatment of Park...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 张丽君卢金萍赵周明郭晓迪沈霞章正赞娄贵川
Owner ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD
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