Data · dataset · 2016
Method development and hydrolytic degradation study of doxofylline by rp-hplc and lc-ms/ms
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A simple, rapid and accurate RP-HPLC method was developed for the determination of doxofylline and photolyticdegradation product.
Description
The method showed a linear response for concentrations in the range of 1-200 g/ml usingacetonitrile: formic acid (90: 10); pH-3.0 as the mobile phase with detection at 274 nm and a flow rate of 1 ml/min and retention time 2.9 min. The method was statistically validated for accuracy, precision, linearity, ruggedness,robustness, forced degradation, solution stability and selectivity.
Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from recovery studies was found to be less than 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis. The hydrolytic degradation product as well as pathway was characterized by LC-MS/MS.RESULT AND DISCUSSION:A sensitive, selective, precise and accurate highperformance liquid chromatographic method of analysis ofdoxofylline in both as bulk drug and in formulation wasdeveloped and validated.
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The mobile phase consisted ofacetonitril: 0.05M formic Acid (90: 10v/v); pH-3.0. Thedetection wavelength was 274nm. This system was found to give the sharp peak for doxofylline (RT-2.9).
The methodwas validated as per ICH guideline (table 1). Stabilityindicating assay method in which hydrolytic stresscondition was used for quantitative estimation ofdoxofylline in tablet formulation and identification ofhydrolytic degradation product The separation of drugfrom its degradation product were optimized by varying theratio &/or nature of organic modifier. Finally method wasdeveloped using same mobile phase composed ofacetonitrile: formic acid (90: 10); pH-3.0, in that both drugand degradation product showing good elution RT-2.9(Doxofylline) and RT-3.68 (Hydrolytic degradationproduct) and m/e-229 (fig 4).
The hydrolytic degradationproduct and pure drug were identified by LC-MS/MS inorder to establish hydrolytic degradation pathway (fig 5 and6).
Links
Where it is published
- Repository landing page figshare.com/articles/dataset/Method_development_and_hydrolytic_degradation… ↗
landing page · from DataCite
- DOI doi.org/10.6084/m9.figshare.3381295.v1 ↗
DOI / persistent id · from DataCite
Documentation and papers
Catalogue records · 2
- DataCite API api.datacite.org/dois/10.6084/m9.figshare.3381295.v1 ↗
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- DataCite Commons commons.datacite.org/doi.org/10.6084/m9.figshare.3381295.v1 ↗
catalogue entry · from DataCite
Topics
- Stated by source
- Basic medicine · Biological sciences · Chemical sciences · Clinical medicine · Health sciences · Medical biotechnology
- From keywords
- Organic chemistry
- Inferred from text
- Mass spectrometry 65% · Tabular 65%
Related
Provenance · 1 source records, 16 field assertions
| Source | Key | Last seen | Raw |
|---|---|---|---|
| DataCite | 10.6084/m9.figshare.3381295.v1 | 15 d ago | JSON v1 |
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| concepts[field].fos:basic-medicine | source · DataCite | connector:datacite@1.0.0 | |
| concepts[field].fos:biological-sciences | source · DataCite | connector:datacite@1.0.0 | |
| concepts[field].fos:chemical-sciences | source · DataCite | connector:datacite@1.0.0 | |
| concepts[field].fos:clinical-medicine | source · DataCite | connector:datacite@1.0.0 | |
| concepts[field].fos:health-sciences | source · DataCite | connector:datacite@1.0.0 | |
| concepts[field].fos:medical-biotechnology | source · DataCite | connector:datacite@1.0.0 | |
| concepts[modality].local:modality:mass-spectrometry | enrichment · DataCite | keyword-concept-rules@1.0.0 | title+description (65%) |
| concepts[modality].local:modality:tabular | enrichment · DataCite | keyword-concept-rules@1.0.0 | title+description (65%) |
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| description | source · DataCite | connector:datacite@1.0.0 | /data/attributes/descriptions |
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