DNPH柱前衍生高效液相色谱法测定啤酒中微量甲醛和乙醛

Determination of trace formaldehyde and acetaldehyde in beer by precolumn derivation high-performance liquid chromatography

目的:探讨DNPH柱前衍生高效液相色谱法测定啤酒中微量甲醛和乙醛的方法。方法:采用蒸馏法处理样品,馏出液于60℃的水浴中衍生20 min,用环己烷提取,最后于液相色谱仪进行分析定量。结果:甲醛、乙醛在0μg/ml～8.0μg/ml浓度范围内,标准曲线线性关系良好,相关系数r分别为0.9998、0.9995;甲醛的相对标准偏差为0.7%～2.9%,乙醛的相对标准偏差为1.3%～3.5%;甲醛的加标回收率为93%～96%,乙醛的加标回收率为93%～102%;甲醛检测结果与国标方法比较无显著性差异(P>0.05)。结论:本方法不但可同时检测啤酒中微量的甲醛和乙醛,具有灵敏度高、选择性好、精密度和准确度好等优点,而且简便、快捷,适合分析大批量检测工作。

Objective：To develop the method for the determination of trace formaldehyde and acetaldehyde in beer by precolumn derivation high -performance liquid chromatography. Methods： The sample was treated by distillation, and the distillate was derived in waterbath at 60℃ for 20 min, then extracted with cyclohexane, finally analyzed by high - performance liquid chromatography for quantification analysis. Results ： The linear ranges of determination for formaldehyde and acetaldehyde were 0 μg/ml.8.0 μg/ml （ r = 0. 9998 ）, 0 μg/ml - 8.0 μg/ml （ r = 0. 9995 ）, respectively. The relative standard derivations for formaldehyde and acetaldehyde were 0.7% - 2.9%, 1.3% -3.5% respectively, and the recoveries of them were 93% -96% , 93% -102% ,respectively. The detection result of formaldehyde had no significant difference with that of national standard method （ P 〉 0.05 ）. Conclusion： The method has the advantages of simplicity, rapidity, high sensitivity, good selectivity, excellent precision and accuracy, which can be used for simultaneous analysis of formaldehyde and acetaldehyde in beer.