Method for separating and measuring acitretin and its genotoxic impurities

A genotoxic and acitretin technology, applied in the field of analytical chemistry, to achieve the effects of high precision and sensitivity, simple and feasible method, and high sensitivity

Active Publication Date: 2018-04-24
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no published method reported for the highly sensitive and rapid separation and determination of acitretin and its genotoxic impurities

Method used

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  • Method for separating and measuring acitretin and its genotoxic impurities
  • Method for separating and measuring acitretin and its genotoxic impurities
  • Method for separating and measuring acitretin and its genotoxic impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Example 1 The method for the separation and determination of genotoxic impurities in acitretin by high performance liquid chromatography

[0065] 1) Prepare a blank solution: take 10ml of tetrahydrofuran, put it in a 100ml measuring bottle, dilute to the mark with methanol, shake well, and you get it;

[0066] 2) Preparation of the test sample solution: take about 40 mg of acitretin, weigh it accurately, put it in a 100 ml measuring bottle, add 10 ml of tetrahydrofuran to dissolve it, and dilute it to the mark with methanol, shake well to obtain (0.4 mg / ml);

[0067] 3) Preparation of genotoxic impurity control stock solution: Accurately weigh 9.45 mg of acitretin methyl ester (batch number: 07032801) and 11.65 mg of acitretin butyl ester (batch number: 07032601), respectively, put them in the same 50ml measuring bottle, add 5ml of tetrahydrofuran Dissolve and dilute to the mark with methanol, shake well to obtain the control stock solution (acitretin (0.189mg / ml) and a...

Embodiment 2

[0077] Embodiment 2 chromatographic system to the degree of separation of acitretin, acitretin methyl ester and acitretin butyl ester

[0078] 1) Prepare a blank solution: take 10ml of tetrahydrofuran, put it in a 100ml measuring bottle, dilute to the mark with methanol, shake well, and you get it;

[0079] 2) Preparation of the test sample solution: take about 40 mg of acitretin, weigh it accurately, put it in a 100 ml measuring bottle, add 10 ml of tetrahydrofuran to dissolve it, and dilute it to the mark with methanol, shake well to obtain (0.4 mg / ml);

[0080] 3) Preparation of genotoxic impurity control stock solution: Accurately weigh 9.45 mg of acitretin methyl ester (batch number: 07032801) and 11.65 mg of acitretin butyl ester (batch number: 07032601), respectively, put them in the same 50ml measuring bottle, add 5ml of tetrahydrofuran Dissolve and dilute to the mark with methanol, shake well to obtain the control stock solution (acitretin (0.189mg / ml) and acitretin b...

Embodiment 3

[0090] Embodiment 3 chromatographic system is to the detection level of acitretin methyl ester and acitretin butyl ester

[0091] 1) Prepare a blank solution: take 10ml of tetrahydrofuran, put it in a 100ml measuring bottle, dilute to the mark with methanol, shake well, and you get it;

[0092] 2) Preparation of the test sample solution: take about 40 mg of acitretin, weigh it accurately, put it in a 100 ml measuring bottle, add 10 ml of tetrahydrofuran to dissolve it, and dilute it to the mark with methanol, shake well to obtain (0.4 mg / ml);

[0093] 3) Preparation of genotoxic impurity control stock solution: Accurately weigh 9.45 mg of acitretin methyl ester (batch number: 07032801) and 11.65 mg of acitretin butyl ester (batch number: 07032601), respectively, put them in the same 50ml measuring bottle, add 5ml of tetrahydrofuran Dissolve and dilute to the mark with methanol, shake well to obtain the control stock solution (acitretin (0.189mg / ml) and acitretin butyl (0.233mg...

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Abstract

The invention belongs to the field of analytical chemistry and relates to a method for separating and measuring acitretin and its genotoxic impurities. The reagent composition used for solid-liquid separation and determination of acitretin and its genotoxic impurities is: an acidic aqueous solution system and an organic solvent; the method for using the above-mentioned reagent composition acitretin and its genotoxic impurities is: take the test sample and dissolve it in Tetrahydrofuran is diluted with a diluent to obtain a sample solution; the mobile phase is prepared; the sample solution is injected into the separation detection system, and the eluent is obtained by eluting and separating the sample solution with the flow; the eluent enters the detection system device measurement. The present invention can completely separate the acitretin and its genotoxic impurities at the same time, the solvent peak in the detection does not interfere with the determination of the acitretin and its genotoxic impurities, and the separation degree is greater than 1.5; and the method is simple, high in sensitivity and short in analysis time, With strong specificity and good reproducibility, it can simultaneously effectively separate and highly sensitively (up to ppm level) determine the content of genotoxic impurities in acitretin raw materials and preparations.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for separating and measuring acitretin and its genotoxic impurities. Background technique [0002] Active pharmaceutical ingredients often contain impurities, including residues and degradation products of raw materials and intermediates used in the synthetic process. Due to their intrinsic activity, some raw materials, intermediates or by-products may be known or suspected mutagens and / or carcinogens. In addition, previously impossible human exposure and risk characterization of genotoxic impurities is now possible with advances in analytical techniques. Assuming that minimization of human exposure is accompanied by minimization of the risk of genotoxic impurities, the availability of high-sensitivity assays is accompanied by increased concerns about the measurement and control of suspected API residues of genotoxic impurities. [0003] Genotoxic impurities (or gen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 沈红梅
Owner CHONGQING HUAPONT PHARMA
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