title: Rapid, simultaneous determination of headspace oxygen and moisture in pharmaceutical packages using muGC.
abstract: The rapid, accurate determination of headspace oxygen and moisture in various pharmaceutical packages is important for both product packaging development and the implementation of new packaging technologies. Current headspace oxygen measurement techniques suffer from serious drawbacks in terms of potential sampling contamination, lengthy analysis times, and large required analysis volumes. In addition, relatively few techniques currently exist for the convenient determination of headspace moisture in packaging systems. Efforts herein focused on the development and application of a new method for the rapid and simultaneous determination of headspace oxygen and moisture in pharmaceutical packages using micro-gas chromatography (muGC). Studies showed that both headspace oxygen and moisture could be simultaneously quantified in <90 s on sample volumes of 50-100 microL by employing muGC with dual chromatographic analysis modules. Sampling issues common to manual syringe-based injections were also alleviated in the current studies by use of the built-in diaphragm pump sampling interface of the portable muGC system. The performance of the analytical approach was evaluated and shown to exhibit excellent linearity, accuracy, and precision for both analytes. High sensitivity for headspace oxygen was demonstrated, allowing for levels of oxygen as low as 0.03% to be accurately quantified. The subject method was applied to measure the headspace oxygen and moisture in pharmaceutical blister packaging and glass vials.
authors.affiliation: Pharmaceutical Research and Development, Merck Research Laboratories, Merck & Co. Inc., West Point, PA 19486, USA.
authors.forename: Hui
authors.initials: H
authors.lastname: Xu
authors.forename: Allen C
authors.initials: AC
authors.lastname: Templeton
authors.forename: Marta
authors.initials: M
authors.lastname: Zwierzynski
authors.forename: Rajiv
authors.initials: R
authors.lastname: Mahajan
authors.forename: Robert A
authors.initials: RA
authors.lastname: Reed
mesh_terms: D002849:Chromatography, Gas / Q000295:instrumentation / Q000379:methods*; D004349:Drug Packaging / Q000379:methods / Q000592:standards*; D004563:Electrochemistry / Q000379:methods; D010100:Oxygen / Q000032:analysis*; D015203:Reproducibility of Results; D013678:Technology, Pharmaceutical / Q000379:methods; D014867:Water / Q000032:analysis
chemical_list: D014867:Water; D010100:Oxygen