摘要
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.
作者
陈蓓
李放
朱峰
刘华良
CHEN Bei LI Fang ZHU Feng LIU Hua-liang(Jiangsu Provincial Center for Disease Control and Prevention, Nanjing 210009,China)
出处
《江苏预防医学》
CAS
2017年第1期22-24,共3页
Jiangsu Journal of Preventive Medicine
基金
江苏省科技厅科技支撑计划项目(BE2010745)
江苏省"十二.五"科教兴卫工程(ZX201109)
关键词
甲醛
乙醛
DNPH柱前衍生
高效液相色谱
Formaldehyde
Acetaldehyde
DNPH Precolumn derivation
High performance liquid chromatography
