关键词: 生物胺, 东北农家酱, 高效液相色谱, 提取, 衍生物萃取

Abstract: In this study, we established a precolumn derivatization-high performance liquid chromatography (HPLC) method and applied it to determine biogenic amines in farmhouse soybean paste from northeastern China. Biogenic amines from samples were extracted with 5% trichloroacetic acid and were precolumn derivatized with dansyl chloride after defatting with n-hexane. A C18 (250 mm×4.6 mm, 5 μm) column was used for the chromatographic separation. Gradient elution was carried out with a mixture of methanol and water at a flow rate of 0.8 mL/min. The biogenic amine content was measured at a wavelength of 254 nm. The results showed that five biogenic amines (histamine, tyramine, β -phenylethylamine, putrescine, and spermidine) from the soybean paste were well separated within 40 min. The linear range for the analytes was 1–50 mg/kg, with correlation coefficients (R2) ≥ 0.99. The detection limits (LODs, RSN = 3) were 0.02–0.06 mg/kg, and the relative standard deviation (RSD) was less than 5%. The average recoveries of the biogenic amines from spiked samples at three concentration levels of 5.0, 10.0 and 15.0 mg/L were between 82% and 105%. The method had a wide linear range, good repeatability and high accuracy, and could allow for quick and simple detection of biogenic amines in northeast farmhouse soybean paste.

Key words: biogenic amines, northeast farmhouse soybean paste, high performance liquid chromatography, extraction, derivative extraction