Development and Validation of a Specific Stability Indicating High Performance Liquid Chromatographic Methods for Related Compounds and Assay of Solifenacin Succinate
Gradient, reverse phase liquid chromatographic methods were developed separately for the related compounds and solifenacin succinate, an active pharmaceutical ingredient used for the treatment of overactive bladder. Gradient LC method was employed for related compounds. The mobile phase-A contains a...
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| Format: | Article |
| Language: | English |
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Wiley
2013-01-01
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| Series: | Journal of Chemistry |
| Online Access: | http://dx.doi.org/10.1155/2013/412353 |
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| author | B. V. Rami Reddy B. Srinivasa Reddy N. V. V. S. S. Raman K. Subhash Reddy C. Rambabu |
| author_facet | B. V. Rami Reddy B. Srinivasa Reddy N. V. V. S. S. Raman K. Subhash Reddy C. Rambabu |
| author_sort | B. V. Rami Reddy |
| collection | DOAJ |
| description | Gradient, reverse phase liquid chromatographic methods were developed separately for the related compounds and solifenacin succinate, an active pharmaceutical ingredient used for the treatment of overactive bladder. Gradient LC method was employed for related compounds. The mobile phase-A contains a 0.01 M phosphate buffer pH: 3.5±0.05 with orthophosphoric acid (88%) and mobile phase-B contains a mixture of acetonitrile and water in the ratio of 90 : 10(v/v). The flow rate was 1.0 mL/minute, column temperature was kept at 35°C, and detection was monitored at 220 nm. In the developed HPLC method the resolution between solifenacin succinate and its closely eluting impurity, that is, solifenacin N-oxide was found to be greater than 3.0. The drug was subjected to stress conditions such as hydrolysis, oxidation, photolysis, and thermal degradation. Considerable degradation was found to occur in only oxidative stress condition. Degradation product formed during oxidative stress condition was found to be impurity-C and it can be identified by LC-MS. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 99.5%. The developed RP-LC method was validated as per ICH guidelines. We also developed LC-MS/MS method for determination and identification of these impurities in solifenacin succinate. |
| format | Article |
| id | doaj-art-cb7a78e8c05143cbb0789707b61f7bd1 |
| institution | Kabale University |
| issn | 2090-9063 2090-9071 |
| language | English |
| publishDate | 2013-01-01 |
| publisher | Wiley |
| record_format | Article |
| series | Journal of Chemistry |
| spelling | doaj-art-cb7a78e8c05143cbb0789707b61f7bd12025-02-03T05:51:18ZengWileyJournal of Chemistry2090-90632090-90712013-01-01201310.1155/2013/412353412353Development and Validation of a Specific Stability Indicating High Performance Liquid Chromatographic Methods for Related Compounds and Assay of Solifenacin SuccinateB. V. Rami Reddy0B. Srinivasa Reddy1N. V. V. S. S. Raman2K. Subhash Reddy3C. Rambabu4Department of Chemistry, Acharya Nagarjuna University, Nagarjunanagar, Guntur 522210, Andhra Pradesh, IndiaHetero Drugs Limited, Balanagar, Hyderabad 500018, Andhra Pradesh, IndiaHetero Drugs Limited, Balanagar, Hyderabad 500018, Andhra Pradesh, IndiaHetero Drugs Limited, Balanagar, Hyderabad 500018, Andhra Pradesh, IndiaDepartment of Chemistry, Acharya Nagarjuna University, Nagarjunanagar, Guntur 522210, Andhra Pradesh, IndiaGradient, reverse phase liquid chromatographic methods were developed separately for the related compounds and solifenacin succinate, an active pharmaceutical ingredient used for the treatment of overactive bladder. Gradient LC method was employed for related compounds. The mobile phase-A contains a 0.01 M phosphate buffer pH: 3.5±0.05 with orthophosphoric acid (88%) and mobile phase-B contains a mixture of acetonitrile and water in the ratio of 90 : 10(v/v). The flow rate was 1.0 mL/minute, column temperature was kept at 35°C, and detection was monitored at 220 nm. In the developed HPLC method the resolution between solifenacin succinate and its closely eluting impurity, that is, solifenacin N-oxide was found to be greater than 3.0. The drug was subjected to stress conditions such as hydrolysis, oxidation, photolysis, and thermal degradation. Considerable degradation was found to occur in only oxidative stress condition. Degradation product formed during oxidative stress condition was found to be impurity-C and it can be identified by LC-MS. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 99.5%. The developed RP-LC method was validated as per ICH guidelines. We also developed LC-MS/MS method for determination and identification of these impurities in solifenacin succinate.http://dx.doi.org/10.1155/2013/412353 |
| spellingShingle | B. V. Rami Reddy B. Srinivasa Reddy N. V. V. S. S. Raman K. Subhash Reddy C. Rambabu Development and Validation of a Specific Stability Indicating High Performance Liquid Chromatographic Methods for Related Compounds and Assay of Solifenacin Succinate Journal of Chemistry |
| title | Development and Validation of a Specific Stability Indicating High Performance Liquid Chromatographic Methods for Related Compounds and Assay of Solifenacin Succinate |
| title_full | Development and Validation of a Specific Stability Indicating High Performance Liquid Chromatographic Methods for Related Compounds and Assay of Solifenacin Succinate |
| title_fullStr | Development and Validation of a Specific Stability Indicating High Performance Liquid Chromatographic Methods for Related Compounds and Assay of Solifenacin Succinate |
| title_full_unstemmed | Development and Validation of a Specific Stability Indicating High Performance Liquid Chromatographic Methods for Related Compounds and Assay of Solifenacin Succinate |
| title_short | Development and Validation of a Specific Stability Indicating High Performance Liquid Chromatographic Methods for Related Compounds and Assay of Solifenacin Succinate |
| title_sort | development and validation of a specific stability indicating high performance liquid chromatographic methods for related compounds and assay of solifenacin succinate |
| url | http://dx.doi.org/10.1155/2013/412353 |
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