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Method for separation and determination of acitretin and genotoxic impurities thereof

A technology of genotoxicity and acitretin, applied in the field of analytical chemistry, achieves the effect of good reproducibility, strong specificity, simple and feasible method

Active Publication Date: 2015-12-09
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 separation and determination of acitretin and genotoxic impurities thereof
  • Method for separation and determination of acitretin and genotoxic impurities thereof
  • Method for separation and determination of acitretin and genotoxic impurities thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Example 1 The method for the separation and determination of genotoxic impurities in acitretin by high performance liquid chromatography

[0064] 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;

[0065] 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);

[0066] 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

[0075] Embodiment 2 chromatographic system to the degree of separation of acitretin, acitretin methyl ester and acitretin butyl ester

[0076] 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;

[0077] 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);

[0078] 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

[0088] Embodiment 3 chromatographic system is to the detection level of acitretin methyl ester and acitretin butyl ester

[0089] 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;

[0090] 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 to the mark with methanol, shake well to obtain (0.4 mg / ml);

[0091] 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 / ml...

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Abstract

Belonging to the field of analytical chemistry, the invention relates to a method for separation and determination of acitretin and genotoxic impurities thereof. A reagent composition for separation and determination of acitretin and genotoxic impurities thereof comprises an acidic aqueous solution system and an organic solvent. The method for separation and determination of acitretin and genotoxic impurities thereof by the reagent composition includes: dissolving a test sample in tetrahydrofuran, and conducting dilution with a diluents to obtain a sample solution; preparing a mobile phase; injecting the sample solution into a separation and detection system, and carrying out elution separation on the sample solution with the mobile phase to obtain an eluent; and sending the eluent into a detector to perform determination. The method provided by the invention can separate acitretin and the genotoxic impurities completely, during detection, the solvent peak has no interference to determination of acitretin and the genotoxic impurities, and the degree of separation is greater than 1.5. Also, the method is simple, and has the advantages of high sensitivity, short analysis time, strong specificity and good reproducibility, and can achieve effective separation and high sensitivity (up to ppm grade) determination of the genotoxic impurity content of acitretin crude drug and preparations thereof.

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 impurity (or genot...

Claims

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Application Information

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