title: Total residue analysis of swabs by ion mobility spectrometry.
abstract: Ion mobility spectrometry (IMS) is a technique attractive for use within the pharmaceutical industry for at-line determination of residues on swabs taken from the surfaces of manufacturing equipment for the purposes of cleaning validation or verification. In this study, the development of a novel IMS method to provide a measurement of total residue present on a swab is described. The technique is based upon quantitation of charged atmospheric gas reactant ion consumption (RIC) within the instrument as a direct measure of the mass of total ionizable residue. Coupled with the conventional analysis of the active pharmaceutical ingredient within a single 2 min analysis, RIC determination provided the benefit of a single measure representative of the presence of multiple residue components or unknown components. To account for differences in response between components of a model drug product (Cymbalta) and its associated cleaning agents, a strategy was proposed to determine a "worst case" total residue test result based on RIC. A limitation of the IMS method was its incompatibility with cleaners containing a high concentration of inorganic components. The methodology provided a range from 5-50 microg per 25 cm(2) surface area and acceptable analyte recovery (50-100%).
authors.affiliation: Lilly Research Laboratories, Eli Lilly and Company, Lilly Corporate Center, Indianapolis, Indiana 46285, USA. strege_mark_a@lilly.com
authors.forename: Mark A
authors.initials: MA
authors.lastname: Strege
mesh_terms: D004345:Drug Industry / Q000295:instrumentation / Q000379:methods / Q000592:standards; D000068736:Duloxetine Hydrochloride; D005079:Excipients / Q000032:analysis / Q000302:isolation & purification; D007477:Ions / Q000032:analysis*; D004364:Pharmaceutical Preparations / Q000032:analysis / Q000302:isolation & purification*; D012680:Sensitivity and Specificity; D013057:Spectrum Analysis / Q000295:instrumentation* / Q000379:methods*; D013876:Thiophenes / Q000032:analysis / Q000302:isolation & purification
chemical_list: D005079:Excipients; D007477:Ions; D004364:Pharmaceutical Preparations; D013876:Thiophenes; D000068736:Duloxetine Hydrochloride