Simultaneous determination of eight underivatized biogenic amines in salted mackerel fillet by ion-pair solid-phase extraction and volatile ion-pair reversed-phase liquid chromatography-tandem mass spectrometry.

A simple and accurate method was developed for the quantitative determination of eight biogenic amines (cadaverine, histamine, 2-phenylethylamine, putrescine, spermidine, spermine, tryptamine, and tyramine) in salted mackerel fillet. The eight biogenic amines in the samples were extracted with 5% trichloroacetic acid and then purified by ion-pair solid-phase extraction using a C18 cartridge and nonafluoropentanoic acid as the volatile ion-pair reagent, without the need for both derivatization and pH adjustment. Subsequently, the eight underivatized biogenic amines were separated and quantified by volatile ion-pair reversed-phase LC-MS/MS using a C18 column with the same volatile ion-pair reagent. The developed method was validated and showed good accuracy with mean recoveries of all the eight analytes in the range of 87-118% at two fortification levels (2.5 and 5 mg/kg). Finally, the proposed method was applied to the analysis of the eight biogenic amines in salted mackerel fillet samples.