溶液捕集-高效液相色谱法测定卷烟主流烟气中主要羰基化合物

HPLC Determination of Major Carbonyl Compounds in Mainstream of Cigarette Smoke with Solvent Trapping

卷烟主流烟气中的羰基化合物用含2,4-二硝基苯肼的乙腈-磷酸溶液为吸收液进行捕集,并在此溶液中使羰基化合物衍生化,所得衍生化产物供高效液相色谱分析。采用Merck LichrosphereRP C_(18)色谱柱进行分离,并用不同配比混合的水-乙腈-四氢呋喃-异丙醇(59+30+10+1)、水-乙腈-四氢呋喃-异丙醇(33+65+1+1)和乙腈的混合液作为流动相进行梯度淋洗,用紫外检测器于波长365 nm处测定。方法的检出限(3S/N)在0.04～0.12μg·g^(-1)之间。方法用于卷烟主流烟气的分析,回收率在75.0%～96.0%之间,测定值的相对标准偏差(n=5)在2.0%～9.3%之间。

Carbonyl compounds in mainstream of cigarette smoke were trapped in a mixture solution of aeetonitrile and H3PO4 （containing 2, 4-dinitrophenylhydrazine）, and derivatized simultaneously therein. The derivatized products obtained were taken for HPLC analysis. Merck Lichrosphere RP C18 column was used as separation column, and mixtures of component A, B and C mixed in various ratios were used in the gradient elution. Component A and B are mixtures of water, acetonitrile, tetrahydrofuran and iso-propand with 2 different ratios of （59＋30＋ 10 ＋ 1 ） and （ 33 ＋ 65 ＋ 1 ＋ 1 ） respectively, and component C is acetonitrile. UV-detection with the wavelength of 365 nm was adopted in the determination. Values of detection limit （3S/N） of the method were found in the range of 0. 04--0.12 μg · g ^-1. The proposed method was applied to the analysis of mainstream of cigarette smoke, giving values of recovery in the range of 75.0%-96.0% and RSD＇s （n=5） in the range of 2.0%-9.3%.