Determination of 9 biogenic amines in aquatic products and meat by high performance liquid chromatography tandem mass spectrometry

ObjectiveTo establish a high-performance liquid chromatography tandem mass spectrometry method for rapid determination of nine biogenic amines in aquatic products （fish， shrimp， shellfish） and meat （pork， beef， mutton） based on non derivatized passing through nsolid-phase extraction pretreatment technology.MethodsAcetonitrile was used to precipitate the protein in the sample， then 0.5% trichloroacetic acid solution was used for extraction. After removing the lipid with n-hexane， lower layer of the sample solution was diluted and purified by passing through a DVB （100 mg/3 mL） solid-phase extraction column. 70% acetonitrile+30% water （containing 100 mmol/L ammonium formate and 0.5% formic acid） and 90% acetonitrile+10% water were used as mobile phase for gradient elution. The target substance was eluted by ACQUITY UPLC® BEH Amide column （1.7 μm， 2.1 mm×100 mm） was used for separation. Electrospray ion source and positive ion multi reaction monitoring mode were used for detection， and internal standard method was used for quantification.ResultsThe linear relationship between putrescine， cadaverine， spermine， and spermine was good within the range of 5-500 ng/mL， while histamine， tyramine， serotonin， phenylethylamine， and β-phenylethylamine were good within the range of 0.5-50 ng/mL， with correlation coefficients r>0.996. The detection limit of putrescine， cadaverine， spermine， and spermidine was 1 mg/kg， and the quantification limit was 3 mg/kg. The detection limit of histamine， tyramine， serotonin， phenylethylamine， and β-phenylethylamine was 0.1 mg/kg， and the quantification limit was 0.3 mg/kg. The spiked recovery rates of low， medium， and high concentrations in aquatic and meat products ranged from 70.6% to 119%， with relative standard deviations less than 10% （n=6）.ConclusionThis method was easy to operate， accurate， reliable， and highly sensitive， and was suitable for the detection of biogenic amines in aquatic products （fish， shrimp， shellfish） and meat （pork， beef， mutton）.