期刊
ANALYTICA CHIMICA ACTA
卷 853, 期 -, 页码 637-646出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.aca.2014.10.004
关键词
Ultra high performance supercritical fluid chromatography; Ultra high performance liquid chromatography; Doping agents; Mobile phase; Make-up solvent
资金
- Charles University in Prague [UNCE 204026/2012]
The conditions for the analysis of selected doping substances by UHPSFC-MS/MS were optimized to ensure suitable peak shapes and maximized MS responses. A representative mixture of 31 acidic and basic doping agents was analyzed, in both ESI+ and ESI- modes. The best compromise for all compounds in terms of MS sensitivity and chromatographic performance was obtained when adding 2% water and 10 mM ammonium formate in the CO2/MeOH mobile phase. Beside mobile phase, the nature of the make-up solvent added for interfacing UHPSFC with MS was also evaluated. Ethanol was found to be the best candidate as it was able to compensate for the negative effect of 2% water addition in ESI- mode and provided a suitable MS response for all doping agents. Sensitivity of the optimized UHPSFC-MS/MS method was finally assessed and compared to the results obtained in conventional UHPLC-MS/MS. Sensitivity was improved by 5-100-fold in UHPSFC-MS/MS vs. UHPLC-MS/MS for 56% of compounds, while only one compound (bumetanide) offered a significantly higher MS response (4-fold) under UHPLC-MS/MS conditions. In the second paper of this series, the optimal conditions for UHPSFC-MS/MS analysis will be employed to screen > 100 doping agents in urine matrix and results will be compared to those obtained by conventional UHPLC-MS/MS. (C) 2014 Elsevier B.V. All rights reserved.
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