Design of experiments guided multivariate calibration for the quantitation of injectable colistimethate sodium by ultra performance liquid chromatography - High resolution mass spectrometry.

Design of experiments guided multivariate calibration for the quantitation of injectable colistimethate sodium by ultra performance liquid chromatography - High resolution mass spectrometry. Talanta. 2020 Dec 01;220:121406 Authors: Dagla I, Tsarbopoulos A, Gikas E Abstract Colistimethate sodium (CMS) is a widely administrated old-generation prodrug for the treatment of the life-threatening infections caused by multi-resistant Gram-negative bacteria. Until now, the quality control procedure of the CMS commercial products is based on microbiological assays. The aim of the study is the development of a chemical analysis methodology based on liquid chromatography - mass spectrometry (LC-MS) that could be used for the quality control of CMS products. The careful optimization of the LC and QToF-MS parameters was deemed crucial, as CMS is known to be a very complex mixture. Thus, a two stage Design of Experiments (DoE) pipeline has been followed, aiming towards the separation of the mixture components. According to the DoE results, a baseline-resolved chromatogram revealing more than 20 compounds was achieved. The separation was performed using a Waters Acquity BEH C8 column employing gradient elution. The mobile phase consisted of aq. ammonium formate 0.005 M (pH 6) (solvent A) and methanol/acetonitrile 79/21 (v/v) (solvent B). A second optimization experiment for the MS signal was employed in order to achieve maximum sensitivity. The sin...
Source: Talanta - Category: Chemistry Authors: Tags: Talanta Source Type: research