title: Assay of histamine by nano-liquid chromatography/tandem mass spectrometry with a packed nanoelectrospray emitter.
abstract: A nano-liquid chromatographic /tandem mass spectrometric (nanoHPLC/MS/MS) method has been developed for the sensitive determination of histamine, a vital neurotransmitter. The method involved pre-column derivatization of histamine with 7-fluoro-4-nitrobenzoxadiazole (NBD-F), thus increasing the hydrophobicity of the analyte and allowing it to be retained and stacked on a nanoelectrospay emitter packed with C18 reversed-phase particles. Sodium 1-heptanesulfonate, added as an ion-pairing reagent in the mobile phase for sample loading, was found to facilitate greatly the analyte retention. The packed nanoelectrospray emitter was easily prepared using fused-silica capillary of 75 microm i.d., and included creating an electrospray emitter tip and then slurry-packing a 5 cm long column with 5 microm silica-based particles. After sample loading, the mobile phase was changed for separation and a characteristic precursor-to-product ion transition, m/z 275 --> 258, was used for the quantification. A linear calibration curve in the range from 1.0-100 ng/mL histamine with an r2 value of 0.9995 was obtained. The detection limit was estimated to be 0.1 ng/mL histamine in water. In a preliminary validation, the method was applied to determine histamine in alcoholic beverages and rat brain tissues.
authors.affiliation: Department of Chemistry, Jackson State University, 1400 Lynch St., Jackson, MS 39204, USA.
authors.forename: Yaru
authors.initials: Y
authors.lastname: Song
authors.forename: Zhe
authors.initials: Z
authors.lastname: Quan
authors.forename: Yi-Ming
authors.initials: YM
authors.lastname: Liu
mesh_terms: D000434:Alcoholic Beverages / Q000032:analysis; D000818:Animals; D001923:Brain Chemistry; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D006632:Histamine / Q000032:analysis* / Q000737:chemistry; D008832:Microchemistry / Q000379:methods; D036103:Nanotechnology / Q000295:instrumentation / Q000379:methods*; D051381:Rats; D021241:Spectrometry, Mass, Electrospray Ionization / Q000295:instrumentation / Q000379:methods*
chemical_list: D006632:Histamine