Design and evaluation of a multi-detection system composed of ultraviolet, evaporative light scattering and inductively coupled plasma mass spectrometry detection for the analysis of pharmaceuticals by liquid chromatography
2008
Pereira, Alberto S. | Schelfaut, Marc | Lynen, Frédéric | Sandra, P (Pat)
Reversed-phase liquid chromatography was coupled to a multi-detection system composed of ultraviolet (UV) detection, evaporative laser scattering detection (ELSD) and inductively coupled plasma mass spectrometry (ICP-MS). By applying the principle of post-column solvent compensation, the organic modifier content was kept constant in ELSD and ICP-MS under gradient elution. Chlorine (³⁵Cl), bromine (⁷⁹Br and ⁸¹Br) and sulfur (³⁴S) were monitored in several pharmaceutical compounds. The limit of quantitation (LOQ) was 80ng/mL for chlorine (chlorpropamide) and 2ng/mL for bromine (bromazepam). Calibration graphs were linear from 1.0μg/mL to 100μg/mL for chlorpropamide (r ² 0.990) and from 10ng/mL to 500ng/mL for bromazepam (r ² 0.996). The low LOQ value for bromine allows to quantify bromine in pharmaceutical samples below the 0.05% level of the active pharmaceutical ingredient.
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