摘要
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.
出处
《中国卫生检验杂志》
北大核心
2012年第8期1783-1784,1787,共3页
Chinese Journal of Health Laboratory Technology
关键词
甲醛
乙醛
2
4-二硝基苯肼
柱前衍生
高效液相色谱
Formaldehyde
Acetaldehyde
2,4dinitrophenylhydrazine
Precolumn derivation
High - performance liquid chromatography