| Identification and characterization of stressed degradation products of metoprolol using LC/Q-TOF-ESI-MS/MS and MS(n) experiments. | |
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MedLine Citation:
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PMID: 21989963 Owner: NLM Status: Publisher |
Abstract/OtherAbstract:
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A rapid, specific and reliable isocratic high-performance liquid chromatography combined with quadrupole time-of-flight electrospray ionization tandem mass spectrometry (LC/Q-TOF-ESI-MS/MS) method has been developed and validated for the identification and characterization of stressed degradation products of metoprolol. Metoprolol, an anti-hypertensive drug, was subjected to hydrolysis (acidic, alkaline and neutral), oxidation, photolysis and thermal stress, as per ICH-specified conditions. The drug showed extensive degradation under oxidative and hydrolysis (acid and base) stress conditions. However, it was stable to thermal, neutral and photolysis stress conditions. A total of 14 degradation products were observed and the chromatographic separation of the drug and its degradation products was achieved on a C(18) column (4.6 × 250 mm, 5 µm). To characterize degradation products, initially the mass spectral fragmentation pathway of the drug was established with the help of MS/MS, MS(n) and accurate mass measurements. Similarly, fragmentation pattern and accurate masses of the degradation products were established by subjecting them to LC-MS/QTOF analysis. Structure elucidation of degradation products was achieved by comparing their fragmentation pattern with that of the drug. The degradation products DP(2) (m/z 153) and DP(14) (m/z 236) were matched with impurity B, listed in European Pharmacopoeia and British Pharmacopoeia, and impurity I, respectively. The LC-MS method was validated with respect to specificity, linearity, accuracy and precision. Copyright © 2011 John Wiley & Sons, Ltd. |
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Authors:
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Roshan M Borkar; B Raju; R Srinivas; Prashant Patel; Satheesh Kumar Shetty |
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Publication Detail:
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Type: JOURNAL ARTICLE Date: 2011-10-12 |
Journal Detail:
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Title: Biomedical chromatography : BMC Volume: - ISSN: 1099-0801 ISO Abbreviation: - Publication Date: 2011 Oct |
Date Detail:
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Created Date: 2011-10-12 Completed Date: - Revised Date: - |
Medline Journal Info:
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Nlm Unique ID: 8610241 Medline TA: Biomed Chromatogr Country: - |
Other Details:
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Languages: ENG Pagination: - Citation Subset: - |
Copyright Information:
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Copyright © 2011 John Wiley & Sons, Ltd. |
Affiliation:
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National Centre for Mass Spectrometry, Indian Institute of Chemical Technology, Hyderabad, 500 607, India; National Institute of Pharmaceutical Education and Research, Balanagar, Hyderabad, 500 037, India. |
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From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine
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