title: Application of (19)  F time-domain NMR to measure content in fluorine-containing drug products.
abstract: It is necessary to show that the active content in the dosage form of drugs is within a certain narrow range of the label claim. In case of fluorinated drugs, the active content can be measured by high field solid state NMR because the excipients lack fluorine. To make NMR reachable to any laboratory, simple to use, and at a low cost, measurement of (19)  F nucleus using a 23 MHz (for (1) H) low field benchtop time-domain (TD) NMR was investigated. Three fluorinated drug products, cinacalcet, lansoprazole, and ciprofloxacin, were chosen for this study. The doses for these drug products range from 15 to 500 mg. The average drug content measured using (19)  F TD-NMR compares well with the reported label claims for the three drugs tested. (19)  F TD-NMR is a simple and non-destructive technique to measure drug content in tablets. In addition, the accessibility and simplicity of the technique makes it an excellent process analytical technology tool for development and manufacturing in the pharmaceutical industry. Copyright © 2015 John Wiley & Sons, Ltd.
authors.affiliation: Department of Attribute Sciences, Amgen Inc., One Amgen Center Drive, Thousand Oaks, CA, 91320-1799, United States.
authors.forename: Maria Victoria
authors.identifier: http://orcid.org/0000-0002-8429-9534
authors.initials: MV
authors.lastname: Silva Elipe
authors.affiliation: Department of Attribute Sciences, Amgen Inc., One Amgen Center Drive, Thousand Oaks, CA, 91320-1799, United States.
authors.forename: Lan
authors.initials: L
authors.lastname: Li
authors.affiliation: Department of Attribute Sciences, Amgen Inc., One Amgen Center Drive, Thousand Oaks, CA, 91320-1799, United States.
authors.forename: Karthik
authors.initials: K
authors.lastname: Nagapudi
authors.affiliation: NMR Service & Consulting, Austin, TX, 78758, United States.
authors.forename: Alan M
authors.initials: AM
authors.lastname: Kook
authors.affiliation: Mestrelab Research S.L., Santiago de Compostela, La Coruňa, 15706, Spain.
authors.forename: Carlos
authors.initials: C
authors.lastname: Cobas
authors.affiliation: Mestrelab Research S.L., Santiago de Compostela, La Coruňa, 15706, Spain.
authors.forename: Isaac
authors.initials: I
authors.lastname: Iglesias
authors.affiliation: Mestrelab Research S.L., Santiago de Compostela, La Coruňa, 15706, Spain.
authors.forename: Chen
authors.initials: C
authors.lastname: Peng
mesh_terms: D002138:Calibration; D000069449:Cinacalcet / Q000737:chemistry; D002939:Ciprofloxacin / Q000737:chemistry; D005461:Fluorine; D017611:Fluorine Compounds / Q000032:analysis*; D007554:Isotopes; D064747:Lansoprazole / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy; D004364:Pharmaceutical Preparations / Q000032:analysis*; D012984:Software; D014961:X-Ray Diffraction
chemical_list: D017611:Fluorine Compounds; D007554:Isotopes; D004364:Pharmaceutical Preparations; D064747:Lansoprazole; D005461:Fluorine; D002939:Ciprofloxacin; D000069449:Cinacalcet
keywords: 19 F; API; NMR; PAT; drug average content; drug product; drug substance; low field NMR; time-domain NMR