摘要
提出了微波辅助衍生-离子液体分散液液微萃取-高效液相色谱法测定发酵酒和饮料中的甲醛。以2,4-二硝基苯肼为衍生试剂,1-辛基-3-甲基咪唑六氟磷酸盐为提取剂,乙腈为分散剂,样品溶液在300 W的微波功率下辐照60s后离心,甲醛衍生物被萃取到离子液体中,用乙腈定容。以SB-C18色谱柱为分离柱,以水-甲醇(2+8)溶液为流动相进行洗脱,检测波长355nm。甲醛的质量浓度在1.00~100μg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)为0.16μg·L-1,测定下限(10S/N)为0.53μg·L-1。对啤酒、葡萄酒、可乐和橙汁4个样品进行加标回收试验,回收率在92.5%~99.1%之间,测定值的相对标准偏差(n=5)在2.6%~7.8%之间。
A method based on HPLC coupled with microwave-assisted derivatization and ionic liquid-based dispersive liquid-liquid microextraction(DLLME)was developed for determination of formaldehyde in fermented wine and beverage.2,4-dinitrophenylhydrazine(DNPH)was used as the derivatization reagent,1-octyl-3-methylimidazolium hexafluorophosphate as extraction solvent,and acetonitrile as disperser.The sample solution was then irradiated at 300 Wof microwave power for 60 sand centrifuged.Formaldehyde derivatives were extracted into the ionic liquid,and then dispersed in acetonitrile for HPLC analysis.The SB-C18 column was used as stationary phase and a mixture of water and methanol as mobile phase.UV-detection was measured at 355 nm.The linear relationship between the peak area and the mass concentration of formaldehyde was in the range of 1.00-100μg·L-1,with detection limit(3S/N)of 0.16μg·L-1 and limit of quantification(10S/N)of 0.53μg·L-1.Tests for recovery were made by adding standard samples to draft beer,wine,cola and orange juice samples,giving recovery rates in the range of 92.5%-99.1% and RSD(n=5)in the range of 2.6%-7.8%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2015年第4期502-505,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
