Determination of flumazenil in plasma by gas chromatography-negative ion chemical ionization mass spectrometry |
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| Authors: | DeMing Song Vladimir Khaykis Kenneth Kohlhof |
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| Affiliation: | 1. Department of Pharmaceutical Technology and Biopharmaceutics, Faculty of Life Sciences, University of Vienna, Vienna 1090, Austria;2. Department of Pharmacognosy, University of Vienna, Vienna 1090, Austria;3. Electron Microscopy Facility, Campus Science Support Facilities GmbH, Dr. Bohr-Gasse 3, Vienna 1030, Austria;4. Research Platform “Characterisation of Drug Delivery Systems on Skin and Investigations of Involved Mechanisms”, University of Vienna, Vienna 1090, Austria;1. Centre of Advanced Study in Marine Biology, Faculty of Marine Sciences, Annamalai University, Parangipettai, 608 502, India;2. CSIR-National Institute of Oceanography, 403 004, Dona Paula, Goa, India;1. Department of Anatomy and Neurobiology, Graduate School of Medicine, Nippon Medical School, 1-1-5 Sendagi, Bunkyo-ku, Tokyo 113-8602, Japan;2. Department of Anesthesiology and Pain Medicine, Graduate School of Medicine, Nippon Medical School, 1-1-5 Sendagi, Bunkyo-ku, Tokyo 113-8602, Japan;1. State Key Laboratory of Pollution Control & Resource Reuse, Tongji University, Shanghai 200092, PR China;2. Institute of Waste Treatment and Reclamation, Tongji University, Shanghai 200092, PR China;3. Centre for the Technology Research and Training on Household Waste in Small Towns & Rural Area, Ministry of Housing and Urban-Rural Development of PR China (MOHURD), PR China;1. Department of Geology, Bates College, Lewiston, ME, United States;2. Graduate School of Oceanography, University of Rhode Island, Narragansett, RI, United States;3. Department of Geosciences, University of Tulsa, Tulsa, OK, United States;4. Ocean Exploration Trust, Narragansett, RI, United States;5. Department of Marine Sciences, Charles Darwin Research Station, Puerto Ayora, Galápagos Islands, Ecuador;6. Pristine Seas, National Geographic Society, Washington, D.C., United States |
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| Abstract: | A gas chromatographic-negative ion chemical ionization mass spectrometric (GC-NCI-MS) method for the determination of flumazenil in plasma is described. The GC of flumazenil (Mr 303) is considered to be difficult as it is readily adsorbed in the GC column. Therefore, preconditioning the GC column with reconstituted extract from plasma and Silyl-8 was required to cover the active sites on the column. Monitoring the maximum mass peak (m/z 275) of the flumazenil resulted in a tenfold enhancement of sensitivity and signal-to-noise ratio (concentration = 1 ng/ml). Isotopically labeled flumazenil-d3 (Mr 306, m/z 278) was used as the internal standard. The detection limit for flumazenil was found to be 0.1 ng/ml with an injection volume of 2 μl. The signal-to-noise ratio was about 10. The routine quantification limit was set at 2 ng/ml for dog plasma and 1 ng/ml for human plasma. The sample volumes in both instances were 1 ml. |
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