title: Trimethylsilyldiazomethane (TMSD) as a new derivatization reagent for trace analysis of selected non-steroidal anti-inflammatory drugs (NSAIDs) by gas chromatography methods.
abstract: Non-steroidal anti-inflammatory drugs (NSAIDs) are among the most common groups of pharmaceuticals detected in environmental matrices. Although several derivatization procedures have been employed in the gas chromatographic analysis of NSAIDs, the application of trimethylsilyldiazomethane has never yet been reported. This work has studied the derivatization of widely used NSAIDs (ibuprofen, ketoprofen and naproxen) by trimethylsilyldiazomethane. Special emphasis was placed on the influence of temperature and reaction time on the reaction yield, and on the determination of the instrumental detection limit. The results are compared with those obtained by methylation using boron trifluoride methanol solution, and by silylation with a mixture of N,O-bis(trimethylsilyl)trifluoroacetamide and trimethylchlorosilane (99:1, v/v) and with N-methyl-N-[tert-butyldimethylsilyl]trifluoroacetamide. The derivatization of ibuprofen, ketoprofen and naproxen by trimethylsilyldiazomethane was shown to be simple, fast, efficient, and suitable for trace analysis (the respective instrumental detection limits for ibuprofen naproxen, and ketoprofen were 2, 4, and 4 ng). Trimethylsilyldiazomethane can be used as an alternative reagent for determining acidic drugs in environmental matrices.
authors.affiliation: Department of Environmental Analysis, Faculty of Chemistry, University of Gdańsk, Sobieskiego 18/19, 80-952 Gdańsk, Poland.
authors.forename: Natalia
authors.initials: N
authors.lastname: Migowska
authors.forename: Piotr
authors.initials: P
authors.lastname: Stepnowski
authors.forename: Monika
authors.initials: M
authors.lastname: Paszkiewicz
authors.forename: Marek
authors.initials: M
authors.lastname: Gołebiowski
authors.forename: Jolanta
authors.initials: J
authors.lastname: Kumirska
mesh_terms: D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000737:chemistry*; D002849:Chromatography, Gas / Q000379:methods*; D003978:Diazomethane / Q000031:analogs & derivatives* / Q000737:chemistry; D057230:Limit of Detection; D008745:Methylation; D014297:Trimethylsilyl Compounds / Q000737:chemistry*
chemical_list: D000894:Anti-Inflammatory Agents, Non-Steroidal; D014297:Trimethylsilyl Compounds; D003978:Diazomethane; C060070:trimethylsilyldiazomethane