亚甲基蓝-高效液相色谱法测定卷烟主流烟气中的硫化氢

Determination of H2S in Main Stream Smoke of Cigarette by Methylene Blue-HPLC Method

建立了亚甲基蓝-HPLC测定卷烟主流烟气中硫化氢含量的方法。考察了卷烟主流烟气中硫化氢的捕集及显色条件。捕集体系为30 mmol/L醋酸锌-20 mmol/L醋酸钠溶液,显色体系为180 mmol/L硫酸、3mmol/L N,N-二甲基对苯二胺二盐酸盐、10 mmol/L硫酸铁铵。衍生产物亚甲基蓝经ZORBAX Eclipse XDB-C18(150 mm×4.6 mm,3.5μm)分离,流动相为甲醇-甲酸-水(45∶1∶55,体积比),流速为0.8 mL/min,DAD检测波长为665 nm。在优化条件下,硫化氢在10.65～532.69μg/L范围内的线性系数为0.999 89。硫离子的加标回收率为96%～98%,RSD为2.4%～3.2%,硫化氢的检出限(MDL)为0.12μg/支。方法可用于卷烟主流烟气中硫化氢的分析测定。

An indirect method for the determination of H=S in main stream smoke of cigarette by HPLC with DAD detector was developed. The influence of coneectration of zinc acetate on trapping effectiveness of H2S in main stream smoke was investigated. The optimal conditions were using 30 mmol/L zinc acetate -20 mmol/L sodium acetate as trapping reagent system, and 180 mmol/L H2SO4 - 3 mmoL/L N, N-dimethyl-p-phenylenediamine dihydroehloride - 10 mmol/L ammonium ferric sulfate as derivation reagent system. The derivative product methylene blue was separated on an Agilent ZORBAX Eclipse XDB -C18（150 mm ×4.6 mm, 3.5 μm）, using a mobile phase composed of methanol - formic acid - water（45 ： 1 ： 55 ） at a flow rate of 0. 8 mL/min. DAD wavelength was set at 665 nm. Under the above optimal conditions, the calibration curve was linear in the concentration range of 10. 65 -532.69 μg/L H2S （0. 1 -5.0 mg/L for methylene blue） with a correlation coefficient of 0. 999 89. The spiked recoveries of S2- were in the range of 96% - 98% with relative standard deviations（RSDs） of 2. 4% -3.2%. The detection limit（MDL） for H2S in main stream smoke of cigarette was 0. 12 μg/cig. The method is simple, rapid and accurate, and could be applied in the determination of H2 S in main stream smoke of cigarette.