对甲氧基苯磺酰氯柱前衍生生物胺的高效液相色谱分离

采用对甲氧基苯磺酰氯作为柱前衍生试剂,RP-HPLC为分析模式,建立了一种新的生物胺衍生化方法,并对葡萄酒中生物胺含量进行检测。通过液质联用对产物进行定性,研究并确定了最适衍生化条件:衍生温度50℃,缓冲液pH 9.0,衍生时间15 min。实验建立了7种生物胺的HPLC分离方法:Beckman ODS柱;流动相A为10 mmol/L的NH4Ac溶液(pH 6.37),B相为乙腈;采用梯度洗脱;流速1 mL/min;检测波长240 nm,室温。

Separation of biogenic amines by high performance liquid chromatography with 4-methoxy benzenesulphonyl chloride as a precolumn derivatization reagent

A novel derivative method for the determination of biogenic amines has been developed by use of 4-methoxy benzenesulphonyl chloride. The derivate production identification was performed by HPLC-MS system. The optimized conditions of derivatization were listed as following: the reaction temperature was 50 ℃;the pH value was 9 and the reaction time was 15 min. The chromatographic conditions were as following: Beckman ODS column (5 μm, 4.6×150 mm),the detection wavelength was 240 nm,the flow rate was 1.0 mL/min;Mobile phase A: 10 mmol/L NH_4Ac (pH 6.37), Mobile phase B: ACN;the gradient protocol was applied. The method has many advantages such as sensitivity, simplicity (pmol), rapidity and stability, which is suitable for the derivatization of biogenic amines and other substances which have amino group.