A new stability-indicating high-performance liquid chromatographic method has been developed for evaluation of degradants, starting materials and process related impurities during the synthesis of sitagliptin phosphate (SIT-P). Separations were achieved on a RP C18 column with linear gradient elution of 0.02 M phosphate buffer at pH 7 and acetonitrile as mobile phase constituents. The flow rate was 1 mL/min and photodiode array detector wavelength was set at 210 nm. Method development was carried in order to elute all starting materials, intermediates during reaction monitoring of stage wise synthesis. Sitagliptin phosphate was subjected for stress conditions like acidic and basic hydrolysis, oxidative, photolytic, neutral and thermal degradation and > 95 % mass balance was achieved, thus ensuring stability indicating capability of the method. Major degradants raised due to acid and base stress were studied by LCMS, identified as Imp-1 (m/z 193.0) and Imp-4 (m/z 234.20), synthesized and subsequently validated along with all other process related impurities as per ICH with respect to specificity, precision, linearity, LOD, LOQ, accuracy, ruggedness and robustness.
Although foam concrete was initially intended to be avoid filler and insulating material, interest in its structural qualities has grown again due to its reduced weight, material savings, and potential for extensive use of waste materials like fly ash. This paper's main objective is to review the present state of knowledge on foam concrete, where sand is partially replaced by glass powder, fly ash, and blast furnace slag in various weights and proportions. The review highlights the necessity for creating new pathways by doing in-depth research on materials, mixture design, and methods to maximise the potential of this material for structural applications.
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