title: Identification of volatile degradants in formulations containing sesame oil using SPME/GC/MS.
abstract: Solid-phase microextraction (SPME), in combination with gas chromatography/mass spectrometry (GC/MS), was used to identify an unknown degradant observed during stability studies of a pharmaceutical formulation containing sesame oil. SPME is a solvent-less, rapid, sensitive, and inexpensive extraction method that minimizes sample preparation. SPME combined with GC is a widely used technique in certain fields, such as food, environmental analysis, forensics, and consumer products, but has only rarely been used for the analysis of pharmaceutical formulations. Hexanal, octanal, 2-octenal, 2-decenal, 2-undecenal, and 2,4-decadienal can be detected and identified by GC/MS, but they cannot be detected by LC/MS due to their volatility and low ionization efficiency under atmospheric pressure ionization conditions. Combining the MS data from the GC/MS with LC/DAD data resulted in the identification of the unknown degradant in the formulation as 2,4-decadienal. The presence of this and other aldehydes was attributed to the oxidative degradation of the unsaturated fatty-acid component in vegetable oils.
authors.affiliation: Pharmaceutics Department, Amgen Inc., One Amgen Center Drive, MS 8-2-D, Thousand Oaks, CA 91320-1799, USA.
authors.forename: Wencan
authors.initials: W
authors.lastname: Chen
authors.forename: Pengzu
authors.initials: P
authors.lastname: Zhou
authors.forename: Kirby C
authors.initials: KC
authors.lastname: Wong-Moon
authors.forename: Nina S
authors.initials: NS
authors.lastname: Cauchon
mesh_terms: D000447:Aldehydes / Q000737:chemistry* / Q000302:isolation & purification; D002214:Capsules / Q000032:analysis; D002626:Chemistry, Pharmaceutical; D002851:Chromatography, High Pressure Liquid; D004340:Drug Contamination; D008401:Gas Chromatography-Mass Spectrometry; D007202:Indicators and Reagents; D010084:Oxidation-Reduction; D012715:Sesame Oil / Q000737:chemistry*; D052617:Solid Phase Microextraction; D013056:Spectrophotometry, Ultraviolet
chemical_list: D000447:Aldehydes; D002214:Capsules; D007202:Indicators and Reagents; C057349:2,4-decadienal; D012715:Sesame Oil