Linalool, nerol, geraniol, citronellol and a-terpineol were phosphorylated and the products purified by adsorption chromatography on XAD-2. High performance liquid chromatography-tandem mass spectrometry (LC-MSMS) analysis using the electrospray ionization technique (ESI) revealed the occurrence of
Evaluation of the sensitivity of miniaturized liquid chromatography-electrospray ionization-mass spectrometry for pharmaceutical analysis
โ Scribed by Martijn Kranendijk; Joop C. M. Waterval; Govert W. Somsen; Gerhardus J. de Jong
- Publisher
- John Wiley and Sons
- Year
- 2005
- Tongue
- English
- Weight
- 453 KB
- Volume
- 28
- Category
- Article
- ISSN
- 1615-9306
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โฆ Synopsis
Abstract
LCโESIโMS is applied frequently in pharmaceutical analysis. The sample amount is generally not restricted, however with LCโESIโMS, a lack of sensitivity may still be observed with standardโbore LC columns in isocratic mode. Therefore, it was investigated whether increased sensitivity could be achieved by using miniaturized LCโESIโMS. Seven columns ranging from 0.1 to 4.6 mm ID were tested using several instrument setups. For proper comparison, a sensitivity gain factor (SGF) was introduced. The SGF expresses the extra sensitivity that may be obtained on top of the normal increase of peak concentration, which can be expected when the column ID is reduced. Desogestrel, mirtazapine, and sugammadex sodium were used as test compounds. For desogestrel and sugammadex sodium, the SGF increased up to a factor of 5โ13 when the column ID was reduced, indicating enhanced ionization efficiencies at lower flow rates. Optimum sensitivity was found for the 0.3 mm column coupled in combination with a microinjection valve and a dedicated low flow rate interface. For mirtazapine, no increase of SGF was observed when the column ID was decreased. Apparently, the ionization efficiency of this compound is not affected by the flow rate and the spray quality.
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