Unlock instant, AI-driven research and patent intelligence for your innovation.

Risperidone raw material or preparation impurity detecting method

A detection method, the technology of risperidone, applied in the field of detection of impurities in risperidone raw materials or preparations, can solve the problems of difficult to accurately measure potential impurities, poor separation effect, poor durability, etc., and achieve a suitable and accurate peak time The effect of detection and method is accurate

Inactive Publication Date: 2017-12-01
天津药物研究院药业有限责任公司 +1
View PDF3 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese Pharmacopoeia adopts the method of isocratic elution, which has poor separation effect on the above 9 known impurities of risperidone, and it is difficult to accurately determine all potential impurities in risperidone raw materials and preparations
The United States and European Pharmacopoeia adopt the gradient elution method, which can separate risperidone and the above-mentioned 9 known impurities, but can only barely reach the baseline separation. The separation degree of impurity D and the main peak is 1.5-1.7. Low separation and poor durability

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Risperidone raw material or preparation impurity detecting method
  • Risperidone raw material or preparation impurity detecting method
  • Risperidone raw material or preparation impurity detecting method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0096] Specific detection method and detection result of related substances of risperidone raw material of the present invention

[0097] Determination method: take the raw material sample of risperidone, add methanol to dissolve and make the test solution containing about 1 mg of risperidone in every 1ml; accurately measure the test solution, accurately measure 1ml, put it in a 100ml measuring bottle, and use Methanol diluted to the mark, shake well, as the control solution. Take an appropriate amount of risperidone reference substance and risperidone impurity A, B, C, D, E, K, Cis-N-O, Trans-N-O, Bicyclo reference substance, weigh them accurately, and dilute with methanol to obtain a concentration of risperidone of about 1mg / ml, impurity concentration of 10μg / ml solution, as a system suitability solution. Take 20 μl of the control solution and inject it into the liquid chromatograph, adjust the sensitivity of the detector so that the peak height of the main component chroma...

Embodiment 2

[0110] Specific detection method and detection result of related substances of risperidone raw material of the present invention

[0111]Determination method: take the raw material sample of risperidone, add methanol to dissolve and make the test solution containing about 1 mg of risperidone in every 1ml; accurately measure the test solution, accurately measure 1ml, put it in a 100ml measuring bottle, and use Methanol diluted to the mark, shake well, as the control solution. Take an appropriate amount of risperidone reference substance and risperidone impurity A, B, C, D, E, K, Cis-N-O, Trans-N-O, Bicyclo reference substance, weigh them accurately, and dilute with methanol to obtain a concentration of risperidone of about 1mg / ml, impurity concentration of 10μg / ml solution, as a system suitability solution. Take 20 μl of the control solution and inject it into the liquid chromatograph, adjust the sensitivity of the detector so that the peak height of the main component chromat...

Embodiment 3

[0123] Specific detection methods and detection results of related substances in the risperidone preparation of the present invention

[0124] Determination method: Take 10 risperidone tablets, grind them evenly in a mortar, accurately weigh an appropriate amount of tablet powder, put it in a volumetric flask, add an appropriate amount of methanol to dissolve it ultrasonically, put it at room temperature, dilute to the mark with methanol, and take the above-mentioned amount by centrifugation. Clear liquid, make the need testing solution that contains about 1mg of risperidone in every 1ml; Accurately measure need testing solution, accurately measure 1ml, put in 100ml measuring bottle, dilute to scale with methanol, shake up, as contrast solution. Take an appropriate amount of risperidone reference substance and risperidone impurity A, B, C, D, E, K, Cis-N-O, Trans-N-O, Bicyclo reference substance, weigh them accurately, and dilute with methanol to obtain a concentration of risp...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Concentrationaaaaaaaaaa
Login to View More

Abstract

The invention provides a risperidone raw material or preparation impurity detecting method. The risperidone raw material or preparation impurity detecting method comprises dissolving risperidone raw materials or preparations, performing gradient elution through high performance liquid chromatography by taking octadecyl silane bonded silica or octyl silane bonded silica as the stationary phase, mixed solution of buffer salt solution and methyl alcohol as the mobile phase A, and mixed solution of methyl alcohol and acetonitrile as the mobile phase B, and then recording the chromatogram within the absorption wavelength of risperidone. The invention provides the high-efficiency liquid chromatography method, and the high-efficiency liquid chromatography method can achieve optimal separation between the risperidone and 9 known impurities and is accurate, effective, good in reproducibility and capable of accurately detecting related substance in the risperidone raw materials and preparations.

Description

technical field [0001] The invention relates to the field of drug analysis, in particular to a method for detecting impurities in risperidone raw materials or preparations. Background technique [0002] Risperidone tablets are a new type of atypical antipsychotic drug developed by Janssen Pharmaceutical Company of Belgium. Its active ingredient risperidone (see the following structural formula) is a benzisoxazole derivative and is a new generation of antipsychotic drugs. A large number of domestic clinical data show that risperidone tablets are superior to traditional antipsychotics in curative effect, effective on positive, negative and emotional symptoms; and have fewer side effects and high safety, which can significantly improve the quality of life of patients. At present, in the raw material synthesis process of risperidone, there are 9 known impurities that may be contained in the final raw material product, including starting materials, intermediates, and degraded im...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): G01N30/02G01N30/38
CPCG01N30/02G01N30/38
Inventor 马超孟策王博张宁王勇杨昕任晓文
Owner 天津药物研究院药业有限责任公司