title: Automated sample preparation for ICP analysis of active pharmaceutical ingredients and intermediates.
abstract: Routine testing of active pharmaceutical ingredients (APIs) for metal residues is an expectation of regulatory bodies such as the FDA (U.S. Food and Drug Administration). Sample preparation techniques are the rate-limiting step in the testing process and can be variable depending on the specific characteristics of the API under test. Simplification and standardization of the routine preparation of inductively coupled plasma spectroscopy sample solutions of organic compounds has been developed using a commercially available robotic workstation. Contamination from the metal components of the instrument and from sample tubes used in the methodology has been studied using a Design of Experiments approach. The optimized method described can be used for the measurement of trace metals in Pharmaceuticals at levels compliant with European and U.S. regulatory requirements.
authors: GlaxoSmithKline, Medicines Research Centre, Stevenage, UK. jon.sims@gsk.com
authors: Jonathan
authors: J
authors: Sims
authors: Andrew
authors: A
authors: Smith
authors: Dharmista
authors: D
authors: Patel
authors: Richard
authors: R
authors: Batchelor
authors: Judith
authors: J
authors: Carreira
mesh_terms: D057205:Automation, Laboratory / Q000379:methods*; D008670:Metals / Q000032:analysis; D004364:Pharmaceutical Preparations / Q000737:chemistry*; D013048:Specimen Handling / Q000379:methods* / Q000592:standards*; D013057:Spectrum Analysis / Q000379:methods*; D014131:Trace Elements / Q000032:analysis
chemical_list: D008670:Metals; D004364:Pharmaceutical Preparations; D014131:Trace Elements