Determination of 15 biogenic amines in fermented alcoholic drink by pass-through solid phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry

A method was established for simultaneous determination of 15 biogenic amines in fermented alcoholic drink using pass-through solid phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), and the methodology was investigated. The results showed that the sample was purified by PRiME HLB column after adding isotopic internal standards, and 15 biogenic amines could be effectively separated by Waters ACQUITY UPLC®BEH C₁₈ chromatographic column (100 mm×2.1 mm, 1.7 μm) with 0.1% formic acid acetonitrile-0.1% formic acid water as the mobile phase. Data was collected by multiple reaction monitoring (MRM) mode. Four biogenic amines (putrescine, N1-acetylspermine, spermidine and 3-methylhistamine) without matrix effect were quantified using external standard method, but the remaining 11 biogenic amines were quantified using internal standard method. The linear relationship of 15 biogenic amines was good within the mass concentration range of 1-100 μg/L, and the correlation coefficients R² were all greater than 0.99. The detection limit and quantification limit were 0.1 mg/L and 0.3 mg/L, respectively. Three different mass concentrations of biogenic amines (0.3 mg/L, 1.0 mg/L, 10.0 mg/L) were added to three types of fermented alcoholic substrates, the average standard recovery rates were 75.6%-109.5%, and the relative standard deviation (RSD) of precision test results was 0.4%-6.4%, indicating that the method was suitable for simultaneous detection of 15 biogenic amines in fermented alcoholic drink. The putrescine, trimethylamine, and tyramine were detected in actual samples of Huangjiu, wine and beer using this method.