International Journal of Pharma and Bio Sciences
ijpbs.net
editorijpbs@rediffmail.com (or) editorofijpbs@yahoo.com (or) prasmol@rediffmail.com
10.22376/ijpbs.2019.10.1.p1-12
Volume 10 Issue 2
2019 (April-June)
Two new degradation products of terizidone: an application of forced degradation study and hyphenated chromatographic technique.
The stability of Terizidone (TERI) drug was determined under different stress conditions in accordance with International Conference on Harmonization (ICH) guidelines Q1A (R2). The chromatogram was developed on precoated silica gel 60F lessThan sub greaterThan 254 lessThan /sub greaterThan TLC plates using ethyl acetate: toluene: methanol (8:1:1 v/v) as a mobile phase. When Terizidone was studied under varied stress conditions, the drug depicted degradation under acidic and oxide stress conditions. However, it was stable under neutral, basic, thermal and photolytic stress conditions. In total, two degradation products (DPs) were formed. NMR and MS/TOF studies were conducted on a mixture of stressed samples to obtain functional group and mass spectral data. The data obtained from the precise mass study was initially used to pattern a complete mass fragmentation pathway of the drug and later for its degradation products. Considering the best possible molecular formula, structures were suggested for each fragment. Two novel degradation products were identified. The study was carried out because of general interest to gather wide-ranging information with respect to the stability of TERI and its degradation pathway. Two novel degradation products (DPs I-II), which got designed during stress study, were separated by HPTLC method. DP-I and DP-II were designed under acidic and oxide stress conditions respectively. To determine structures of unknown degradation products, drug, and all the degradants were subjected for IR and MS/TOF study. From presented mass spectral data, complete degradation pathways for drug and degradation products were recognized. Subsequently our knowledge, such type of work is described for the first time to lead with force degradation studies and their aspects.
PALLAVI M PATIL AND AHMED ALALAIWE
Terizidone; HPTLC; Validation; Degradation pathway; Mass spectrometer; NMR
58-70