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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 investigate the method for determination of trace formaldehyde and acetaldehyde in beer by high performance liquid chromatography (DNPH) pre-column derivatization. Methods: The sample was treated by distillation. The distillate was derivatized in water bath at 60 ℃ for 20 min, extracted with cyclohexane and finally analyzed by liquid chromatography. Results: The calibration curve of formaldehyde and acetaldehyde showed a good linearity in the range of 0μg / ml ~ 8.0μg / ml with the correlation coefficients r of 0.9998 and 0.9995 respectively. The relative standard deviations of formaldehyde were 0.7% -2.9% The standard deviation was 1.3% ~ 3.5%, the recovery of formaldehyde was 93% ~ 96%, and the recovery of acetaldehyde was 93% ~ 102%. The formaldehyde test results showed no significant difference with the national standard method (P> 0.05). Conclusion: This method not only can detect trace amounts of formaldehyde and acetaldehyde in beer at the same time, but also has the advantages of high sensitivity, good selectivity, good precision and accuracy, and is simple, rapid and suitable for the analysis of large quantities of testing.