高效液相色谱法同时测定保健酒中的微量甲醛和乙醛

Simultaneous determination of trace formaldehyde and acetaldehyde in nutritional health care wine by high performance liquid chromatography

目的探讨柱前衍生高效液相色谱法(HPLC)测定保健酒中微量甲醛和乙醛的方法。方法样品经水蒸气蒸馏,与2,4-二硝基苯肼(DNPH)在60℃水浴中衍生成为苯腙,经二氯甲烷提取后挥干,加乙腈∶水(1∶1V/V)复溶,取滤液采用HPLC进行检测。以乙腈+水为流动相,梯度洗脱。结果甲醛、乙醛在0.5~10.0mg/L浓度范围内,线性关系良好,相关系数(r)>0.999。平均回收率甲醛为96.9%~103.3%,乙醛为99.8%~106.0%;相对标准偏差(RSD)甲醛为1.8%~6.3%,乙醛为1.6%~5.6%;最低检出限甲醛、乙醛分别为0.03、0.05mg/L。结论建立的方法灵敏度较高,且简便、准确,适用于快速测定深色发酵类保健酒中甲醛和乙醛的含量。

Objective To develop an analysis for trace formaldehyde and acetaldehyde in health care wine by high performance liquid chromatography（HPLC）after precolumn derivatization.Methods The sample was incubated with 2,4-dinitrophenylhydrazine（DNPH）to derive phenylhydrazone in water-bath at 60℃after steam distillation,which was extracted by dichloromethane extraction and dried by evaporation.The residue was redissolved in acetonitrile：water（1∶1）,the filtrate was subjected for HPLC analysis,using acetonitrile＋water as mobile phase for gradient elution.Results The linear ranges for formaldehyde and acetaldehyde were 0.5-10.0mg/L（r0.999）.The average recovery rates of formaldehyde was 96.9%-103.3%;the average recovery rates of acetaldehyde was 99.8%-106.0%.The relative standard deviation of formaldehyde was 1.8%-6.3%;the relative standard deviation of acetaldehyde was 1.6%-5.6%.The limit of detection of formaldehyde and acetaldehyde was 0.03mg/L and 0.05mg/L,respectively.Conclusion The method is highly sensitive,convenient,accurate and suitable for rapid determination of formaldehyde and acetaldehyde in dark fermented wines.