作者: Ruth A. Perez , Nils Rehmann , Sheila Crain , Patricia LeBlanc , Cheryl Craft
DOI: 10.1007/S00216-010-4161-2
关键词: Spectroscopy 、 Ampoule 、 Chromatography 、 Nuclear magnetic resonance spectroscopy 、 Anhydrous 、 Mass spectrometry 、 Methanol 、 Chemistry 、 Stock solution 、 Azaspiracid
摘要: The production and certification of a series azaspiracid (AZA) calibration solution reference materials is described. Azaspiracids were isolated from contaminated mussels, purified by preparative liquid chromatography dried under vacuum to the anhydrous form. purity was assessed chromatography–mass spectrometry nuclear magnetic resonance spectroscopy. final concentration each AZA in CD3OH stock determined quantitative NMR This then diluted very accurately degassed, high methanol 1.47 ± 0.08 μmol/L for CRM-AZA1, 1.52 0.05 CRM-AZA2, 1.37 0.13 CRM-AZA3. Aliquots dispensed into argon-filled glass ampoules, which immediately flame-sealed. solutions are suitable method development, validation, or mass instrumentation quality control shellfish monitoring programs.