高效液相色谱法测定烟用酒精中羰基化合物

摘要

A method of HPI.C for the simultaneous determination of 7 carbonyl compounds, i. e., formaldehyde, acetaldehyde, acetone, acraldehyde, crotonaldehyde, 2-butanone and butyraldehyde, in ethanol used for cigarettes was proposed. In an acidic medium, the sample was derivatized with the derivatizing reagent, 2,4-dinitrophenylhydrazine (2,4-DNPH). The derivatives of 7 carbonyl compounds were used for HPLC analysis, using Phenomenex Luna 5u C18 column as stationary phase and mixtures of acetonitrile and water mixed in different ratios as mobile phases in gradient elution. PAD at the wavelength of 352 nm was adopted in the determination. Linear relationships between values of peak area and concentration of 7 earbonyl compounds were obtained in the definite ranges, with detection limits (3S/N) in the range of 3.9-9. 9μg ·L^-1. Using samples of blank ethanol as matrixes, tests for recovery were made by standard addition method, and values of recovery obtained were in the range of 97. 0%-99.0%, with values of RSD's (n=5) in the range of 0. 2%--2. 1%.%提出了高效液相色谱法同时测定烟用酒精中7种羰基化合物（甲醛、乙醛、丙酮、丙烯醛、巴豆醛、2-丁酮和丁醛）含量的方法。烟用酒精在酸性条件下经2，4-二硝基苯肼（2，4-DNPH）衍生化，所得衍生物用Phenomenex Luna5uC18色谱柱分离，用不同体积比的乙腈和水混合作流动相梯度洗脱，用二极管阵列检测器于波长352nm处检测。7种羰基化合物的质量浓度分别在一定范围内与其峰面积呈线性关系，检出限（3S／N）在3．9～9．9μg·L^-1之间。以空白烟用酒精为基体进行加标回收试验，回收率在97．0％～99．0％之间，相对标准偏差（n=5）在0．2％～2．1％之间。