分散液相微萃取/高效液相色谱法同时测定啤酒中3种酮类老化物质

Simultaneous Determination of Three Keto Ageing Compounds in Beer by DLLME/HPLC

建立了分散液相微萃取(DLLME)/高效液相色谱(HPLC)同时测定啤酒中双乙酰、2,3-戊二酮和β-大马酮3种主要酮类老化物质的方法。确定了双乙酰和2,3-戊二酮的衍生化反应条件和3种目标组分同时检测的高效液相色谱条件,在15 min内实现了对3种酮类老化物质的分离和检测;优化了分散液相微萃取的实验条件,使3种目标组分得到同时提取和富集,各组分的富集倍数分别为45、63、121倍。所建立的3种组分的工作曲线相关系数良好(r为0.999 6～0.999 9),线性范围可达3～4个数量级,检出限(S/N=3)为0.3～0.9μg/L,样品的加标回收率为86%～97%,相对标准偏差为2.4%～4.8%。

A method for the simultaneous determination of three main keto ageing compounds, such as diacetyl, 2, 3-pentanedione and β-damascone, in beer by dispersive liquid -liquid microextraction/high performance liquid chromatography was proposed. Derivatization conditions of diacetyl and 2, 3-pentanedione and high performance liquid chromatography conditions of the three target components were established. The separation and detection of three keto ageing compounds were performed in 15 min. The conditions of dispersive liquidliquid microextraction were studied, and the enrich-ent factors of three compounds were 45, 63 and 121, respectively. Good linearities were obtained for three compounds with correlation coefficients of 0. 999 6 - 0. 999 9, and the linear range is greater than or equal to 103. The detection limits（S/N =3） were in the range of 0.3 -0. 9 μg/L. The average recoveries of real samples were in the range of 86% - 97% with RSDs of 2. 4% - 4. 8%.