以4-氟-7-硝基-2,1,3-苯并氧杂恶二唑(NBD-F)为衍生化试剂,建立了食品中5种痕量生物胺(色胺、组胺、酪胺、亚精胺、精胺)的毛细管电色谱-激光诱导荧光检测(CEC-LIF)分析方法.采用50 mmol/L 硼酸盐缓冲溶液(pH 8.0)作为衍生介质,在75 ℃条件下对生物胺进行衍生化反应25 min.生物胺衍生产物的最优色谱条件:固定相为C18毛细管电色谱柱,流动相为乙腈-乙酸铵(20 mmol/L, pH 8.0)(75∶25, v/v),辅助压力为6.9 MPa,分离电压为-8 kV,流速为0.03 mL/min.实验结果表明,生物胺的检出限(LOD, S/N=3)为0.1~1.0 μg/L,加标回收率为78.3%~113.9%.该方法可成功用于加工和发酵食品中生物胺的测定,结果与传统HPLC法的检测结果无显著性差异,且检出限更低、分析速度更快,对于食品中痕量污染物的残留监测具有应用价值.
A rapid and sensitive method was established for the analysis of biogenic amines (tryptamine, histamine, tyramine, spermidine and spermine) in foods by capillary electrochromatography (CEC) coupled with laser induced fluorescence (LIF) detection, using 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) as the derivatization reagent.The biogenic amines were derivatized by NBD-F with 50 mmol/L borate buffer solution (pH 8.0) at 75 ℃ for 25 min.The obtained derivatives of biogenic amines were separated on a packed C18 capillary column with a mobile phase consisting of acetonitrile-ammonium acetate (20 mmol/L, pH 8.0) (75∶25, v/v) and the flow rate of 0.03 mL/min.A supplementary pressure of 6.9 MPa and a separation voltage of -8 kV were applied.The limits of detection (LODs, S/N=3) were 0.1-1.0 μg/L, with spiked recoveries of 78.3%-113.9%.The method could be applied to detect biogenic amines in processed and fermented foods.Statistical comparison of the results with those of the reference HPLC method showed good agreement.It reveals some advantages on the sensitivity and analysis speed, which are significant to trace residue analysis of biogenic amines in foods.
参考文献
| [1] | Palermo, C.;Muscarella, M.;Nardiello, D.;Iammarino, M.;Centonze, D..A multiresidual method based on ion-exchange chromatography with conductivity detection for the determination of biogenic amines in food and beverages[J].Analytical and bioanalytical chemistry,20132/3(2/3):1015-1023. |
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