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Analysis method for determining lubiprostone test sample related substances

A lubiprostone and analytical method technology, applied in the field of drug analysis, can solve problems such as structural instability of lubiprostone

Active Publication Date: 2020-06-30
NANJING CHIA TAI TIANQING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the structure of lubiprostone itself is unstable, and there will be tautomerism between compound L and compound L':

Method used

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  • Analysis method for determining lubiprostone test sample related substances
  • Analysis method for determining lubiprostone test sample related substances
  • Analysis method for determining lubiprostone test sample related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Embodiment 1 related substance determination method

[0082] Get an appropriate amount of lubiprostone test sample, accurately weighed, dissolve and dilute with acetonitrile to make a solution containing about 5 mg in every 1ml, as the test solution; get an appropriate amount of lubiprostone reference substance, accurately weighed, use Acetonitrile was dissolved and diluted to make a solution containing about 10 μg per 1 ml as a reference solution; another appropriate amount of lubiprostone, compound of formula I, compound of formula II, compound of formula III, compound of formula IV and compound of formula V , accurately weighed, dissolved with acetonitrile and diluted respectively to make a solution containing about 5 mg of lubiprostone in every 1 ml, a solution containing about 5 μg of compound of formula I in every 1 ml, a solution of about 5 μg of compound of formula II in every 1 ml, The solution containing about 5 μg of the compound of formula III in each 1 ml, ...

Embodiment 2

[0091] Embodiment 2 related substance determination repeatability experiment

[0092] Get an appropriate amount of the test sample, add acetonitrile to dissolve and dilute to make a solution containing about 5 mg per 1 ml, as the test sample solution, prepare six parts in parallel, according to the method described in Example 1, sample injection analysis, and calculate with the self-control method Each impurity and the total impurity content were used to examine the repeatability of the method. The measurement results are shown in the table below:

[0093] Table of repeatability test results

[0094] sample 1 2 3 4 5 6 Compound of formula III (%) 0.04 0.04 0.04 0.04 0.04 0.05 Formula I compound (%) not detected not detected not detected not detected not detected not detected Formula IV compound (%) not detected not detected not detected not detected not detected not detected Formula II compound (%) not detected...

Embodiment 3

[0096] Embodiment 3 related material intermediate precision experiment

[0097] According to the method described in Example 1, two analysts were respectively on two different high-performance liquid chromatographs, measured according to the related substance determination method, and counted each impurity and the total impurity content. The results of the intermediate precision of the method for determination of related substances are shown in the table below:

[0098] Table of intermediate precision results for related substances

[0099]

[0100] It can be seen from the above table that the results of the intermediate precision show that the content of the compound of formula III is 0.03% to 0.05%, the maximum single impurity content is: 0.03% to 0.04%, and the total impurity content is: 0.07% to 0.10%. The intermediate precision of this method is good.

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Abstract

The invention provides an analysis method for determining lubiprostone test sample related substances, which adopts reversed-phase high-performance liquid chromatography to separate and determine a lubiprostone compound, a compound shown as a formula I, a compound shown as a formula II, a compound shown as a formula III, a compound shown as a formula IV and a compound shown as a formula V. According to the method, the solvent does not interfere with impurity detection, the specificity of the method is good, the detection method is simple, convenient, high in sensitivity, good in repeatabilityand good in accuracy, qualitative and quantitative analysis of related substances of a test sample can be rapidly and accurately carried out, and the controllability of lubiprostone quality is guaranteed.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a high performance liquid chromatography analysis method for lubiprostone related substances. [0002] technical background [0003] Lubiprostone (Compound L) It is a limited chloride ion channel activator, which can selectively activate the type 2 chloride ion channel located on the luminal cell membrane at the tip of the gastrointestinal tract epithelium, increase the secretion of intestinal fluid and the motility of the intestinal tract, thereby increasing defecation, FDA has Lubiprostone is approved for the treatment of chronic idiopathic constipation in adults, constipation-predominant irritable bowel syndrome in adult women, and constipation associated with opioid use. However, the structure of lubiprostone itself is unstable, and there will be tautomerism between compound L and compound L': [0004] [0005] In the quality control of lubiprostone test product, in the exis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 王丽娟胡越吴晶王华萍兰公剑柴雨柱徐丹朱春霞田舟山
Owner NANJING CHIA TAI TIANQING PHARMA
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