反相-高效液相色谱法同时检测食品中4种α-二羰基化合物

Simultaneous determination of four α-dicarbonyls in food by RP-HPLC-DAD

建立了4种α-二羰基化合物[3-脱氧奥苏糖（3-DG）、乙二醛（GO）、丙酮醛（MGO）、2,3-丁二酮（2,3-BD）]的反相-高效液相色谱检测方法。首先将α-二羰基化合物与邻苯二胺反应生成喹喔啉衍生物（温度为60℃,p H=9.00,反应时间4h）,然后用HPLC检测。色谱柱为Agilent ZORBAX SB-Aq（4.6mm×250mm,5μm）,流速为0.7m L/min,流动相A为0.1%醋酸水溶液,B为甲醇,线性梯度洗脱程序为：0-35min,B 35%-70%;35-40min,B 70%-35%;40-50min,B 35%。30min内4种喹喔啉衍生物得到了较好的分离。方法学考察结果表明该HPLC方法具有很好的重现性和准确性,能够满足定量分析的要求。同时该方法适用于蜂蜜、食醋、凉果、咖啡中4种α-二羰基化合物含量的检测。

A RP-HPLC quantitative method for simultaneous determination of four α-dicarbonyls, 3- deoxyglucosulose （ 3 - DG ） , glyoxal （ GO ） , methylglyoxal （ MGO ）, and 2,3 - butanedione （ 2,3 - BD ）, was established, cc-dicarbonyls were reacted with phenylenediamine to form quinoxaline derivative at 60℃,pH9.00 for 4h. The derivatives were separated on an Agilent column ZORBAX SB-Aq （4,6mm×250mm, 5μm） using 0.1%acetic acid aqueous solution（A） and methanol（B） as mobile phase for the following stepwise gradient elution ： 35% -70% （B） in 0 -35min, 70% -35% （B） in 35-40min, 35% （ B ） in 40 -50min, the flow rate was 0.7mL/min. The results showed that the four quinoxaline derivatives were well separated within 30min. This method could meet the quantitative analysis because of its good reproducibility and accuracy confirmed by methodology.It was also well applied in the determination of four α-dicarbonyls in honey,vinegar,preserved fruit, and coffee.