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.

Nano and rapid resolution liquid chromatography–electrospray ionization–time of flight mass spectrometry to identify and quantify phenolic compounds in olive oil

“…For coupling nanoLC to MS, several nanospray interfaces have been tested (sheath liquid and sheathless), some of them commercially available and, in many occasions, homemade [6,17].…”

Recent applications in nanoliquid chromatography

“…(see Table 3), although not so often like in the ones previously discussed. Song et al [144] developed a nano-LC-MS method using a nanoelectrospray interface for the determination of the neurotransmitter histamine in water and also, as a preliminary validation, in alcoholic beverages and rat brain tissues. For this purpose, a 75 lm id column was packed with C 18 particles of 5 lm and a mobile phase composed of water, ACN, formic acid, and 1-heptanesulfonic acid as ion-pairing reagent was used.…”

Quantitation of cardioexcitatory Asn‐D‐Trp‐Phe‐NH2 diastereomers in Aplysia's central nervous system by nanoscale liquid chromatography‐tandem mass spectrometry

“…26 A piece of 20 cm long capillary (75-µm ID) was held vertically with a weight attached to the lower end. The capillary was heated at a spot close to its lower end using a burner.…”