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2. Assessment of labelled products with different radioanalytical methods: study on F-fluorination reaction of 4-[F]fluoro-N-[2-[1-(2-methoxyphenyl)-1-piperazinyl]ethyl-N-2-pyridinyl-benzamide ( p-[F]MPPF).

Author

Koivula, Teija, Laine, Jaana, Lipponen, Tiina, Perhola, Outi, Kämäräinen, Eeva-Liisa, Bergström, Kim, and Solin, Olof

Subjects
FLUORINATION, SEROTONIN agonists, BENZAMIDE, LIGANDS (Chemistry), MICROWAVE heating, CHROMATOGRAPHIC analysis, HIGH performance liquid chromatography, MASS spectrometry, LIQUID chromatography
Abstract

The serotonin receptor 5-HT ligand 4-[F]fluoro-N-[2-[1-(2-methoxyphenyl)-1-piperazinyl]ethyl-N-2-pyridinyl-benzamide ( p-[F]MPPF) was produced by a simplified method of Le Bars et al. Traditional oil bath heating was compared to microwave heating. Various radioanalytical methods, radio-Thin Layer Chromatography (TLC), High Pressure Liquid Chromatography (HPLC) and Mass Spectrometry (MS), were compared in the evaluation of the labelled product(s). The crude reaction mixture consisted of p-[F]MPPF and 2-4 radioactive by-products eluting after the product fraction, and the reverse-phase HPLC method failed occasionally to separate p-[F]MPPF from the radioactive by-product with close retention time. The heating method had no significant effect on the composition of labelled by-products. In LC-(ESI)-MS analysis of p-[F]MPPF the labelled product was identified with m/ z ratio of 435 ([M + H]). The other HPLC fractions were measured to have following m/ z ratios: (1) 327; 349; (675) (2) 402; 407/408; (791) and (3) 436, suggesting different kind of decomposition of the labelled product and/or the inactive precursor. The ion trap mass spectrometer was sufficient for the qualitative analysis of p-[F]MPPF. However, differentiation of by-products arising from the decomposition of p-[F]MPPF or from its precursor p-MPPNO proved to be challenging. [ABSTRACT FROM AUTHOR]

Published
2010
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3. Assessment of labelled products with different radioanalytical methods: study on 18F-fluorination reaction of 4-[18F]fluoro-N-[2-[1-(2-methoxyphenyl)-1-piperazinyl]ethyl-N-2-pyridinyl-benzamide (p-[18F]MPPF)

Author

Kim Bergström, Tiina Lipponen, Jaana Laine, Olof Solin, Outi Perhola, Teija Koivula, Eeva-Liisa Kämäräinen, Koivula, Teija, Laine, Jaana, Lipponen, Tiina, Perhola, Outi, Kämäräinen, Eeva-Liisa, Bergström, Kim, Solin, Olof, University of Helsinki, Department of Chemistry, University of Helsinki, Department of Chemistry (-2009), University of Helsinki, Laboratory of Radiochemistry (Dep. of Chemistry) (-2009), and University of Helsinki, Faculty of Pharmacy

Subjects
Health, Toxicology and Mutagenesis, education, 116 Chemical sciences, Mass spectrometry, High-performance liquid chromatography, 030218 nuclear medicine & medical imaging, Analytical Chemistry, 03 medical and health sciences, chemistry.chemical_compound, 0302 clinical medicine, MPPF, Liquid chromatography–mass spectrometry, Radiology, Nuclear Medicine and imaging, Benzamide, Hplc method, Spectroscopy, Radioanalytical methods, Chromatography, Chemistry, Radiolabelling, Public Health, Environmental and Occupational Health, Pollution, Fluorine-18, LC-MS, Nuclear Energy and Engineering, Microwave heating, Retention time, 030217 neurology & neurosurgery
Abstract

The serotonin receptor 5-HT1A ligand 4-( 18 F) fluoro-N-(2-(1-(2-methoxyphenyl)-1-piperazinyl)ethyl-N- 2-pyridinyl-benzamide (p-( 18 F)MPPF) was produced by a simplified method of Le Bars et al. Traditional oil bath heating was compared to microwave heating. Various radioanalytical methods, radio-Thin Layer Chromatogra- phy (TLC), High Pressure Liquid Chromatography (HPLC) and Mass Spectrometry (MS), were compared in the evaluation of the labelled product(s). The crude reaction mixture consisted of p-( 18 F)MPPF and 2-4 radioactive by-products eluting after the product fraction, and the reverse-phase HPLC method failed occasionally to sepa- rate p-( 18 F)MPPF from the radioactive by-product with close retention time. The heating method had no significant effect on the composition of labelled by-products. In LC-(ESI)-MS analysis of p-( 18 F)MPPF the labelled product was identified with m/z ratio of 435 ((M ? H ? )). The other

Published
2010

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