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Analysis of microso...
Analysis of microsomal metabolic stability using high-flow-rate extraction coupled to capillary liquid chromatography-mass spectrometry
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- Lavén, Martin (författare)
- Uppsala universitet,Kemiska institutionen,Analytisk kemi
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- Markides, Karin E. (författare)
- Uppsala universitet,Kemiska institutionen,Analytisk kemi
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Långström, Bengt (författare)
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(creator_code:org_t)
- 2004
- 2004
- Engelska.
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Ingår i: Journal of Chromatography B. ; :806, s. 119-126
- Relaterad länk:
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https://urn.kb.se/re...
Abstract
Ämnesord
Stäng
- A method described for on-line high-speed extraction of microsomal samples and analysis by capillary liquid chromatography - mass spectrometry (LC-MS) for the determination of metabolic stability in connection with the development of positron emission tomography (PET) tracers. the method allowed direct injections of large sample volumes at a fast extraction rate, providing a gain in both sensitivity and sample preparation time. The calibration curve of the test compound flumazenil (Ro 15-1788) was linear in the concentration range of 1-150 nM, with a correlation coefficient exceeding 0.999. The accuracy of the method ranged from 98 to 101%. A high precision was obtained, with mean intra-assay and inter-assay relative standard deviations of at most 1.4 and 1.5%, respectively, for quality control (QC) samples. The extraction efficiency was determined to be 99.4%, the total recovery 96% and the carryover to <0.23%. Extractions were performed in a concentration interval of 30-300 nM without any sign of column overload. The method was successfully used for determining the microsomal metabolic stability of flumazenil. As a result, the described analysis system is currently used for metabolic screening of PET tracer candidates in our laboratory.
Nyckelord
- High-flow-rate extraction
- Metabolic stability
- Positron emission tomography
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