Liquid Chromatography-Particle Beam Electron Ionization Mass Spectrometry Method for Analysis of Botanical Extracts: Evaluation of Ephedrine Alkaloids in Standard Reference Materials
| Autor: | Joaudimir Castro, M. V. B. Krishna, R. K. Marcus |
|---|---|
| Rok vydání: | 2010 |
| Předmět: |
Pharmacology
Ephedra sinica Chromatography ved/biology Chemistry ved/biology.organism_classification_rank.species Methylephedrine Pseudoephedrine Mass spectrometry High-performance liquid chromatography Analytical Chemistry Standard addition medicine Environmental Chemistry Ephedrine Agronomy and Crop Science Electron ionization Food Science medicine.drug |
| Zdroj: | Journal of AOAC INTERNATIONAL. 93:1788-1797 |
| ISSN: | 1944-7922 1060-3271 |
| Popis: | The preliminary validation of a high-performance liquid chromatography particle beam mass spectrometry method (HPLC-PB/MS) with electron impact ionization source for analysis of botanical extracts is presented. The LC-PB/MS system was evaluated for the analysis of ephedrine alkaloids using ephedra-containing National Institute of Standards and Technology dietary supplement standard reference materials (SRMs) 3241 Ephedra Sinica Stapf Native Extract and 3242 Ephedra Sinica Stapf Commercial Extract. The ephedrine alkaloids were separated by reversed-phase chromatography using a phenyl column at room temperature. A linear gradient method with a mobile phase composition varying from 5:95 [MeOH:0.1 trifluoroacetic acid (TFA) in water] to 20:80 (MeOH:0.1 TFA in water) at a flow rate of 1.0 mL/min, with an analysis time of less than 20 min, was used. The source block temperature was evaluated to determine the optimal operating conditions by monitoring the intensities and fragmentation patterns of the ephedrine alkaloids. Ephedrine and N-methylephedrine were taken as a representative of the test alkaloids. The LODs on the sub-nanogram level were achieved, with ephedrine, pseudoephedrine, and methylephedrine in the SRMs quantified by a standard addition method with recoveries of 86 and RSDs of 14 (N = 3). |
| Databáze: | OpenAIRE |
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