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衍生-顶空气相色谱法测定烟用水基胶中的甲醛、乙醛和丙酮

Analysis of formaldehyde, acetaldehyde and acetone in water-based adhesives for cigarette by derivatization-headspace gas chromatography

  • 摘要: 为准确测定烟用水基胶中甲醛、乙醛和丙酮的残留量,通过对顶空进样条件和气相色谱参数进行优化,建立了一种测定烟用水基胶中甲醛、乙醛和丙酮的衍生-顶空气相色谱(HS-GC)方法。水基胶样品加水后,室温下振荡萃取;离心后移取上清液到顶空瓶,加入PFBHA溶液并立即密封,涡旋混匀;样品溶液经70℃、50 min顶空加热后,用HP-5色谱柱分离、氢火焰离子化检测器检测和外标法定量。结果表明:①甲醛、乙醛和丙酮的检出限和定量限分别为0.013~0.023和0.042~0.075 mg/kg,回收率为95.3%~106.0%,相对标准偏差(RSD)≤6.1%;②采用该方法对实际水基胶样品进行了检测,检测结果与行业标准高效液相色谱(HPLC)方法相吻合。该方法简单、准确、环境友好,适用于烟用水基胶中的甲醛、乙醛和丙酮的常规检测。

     

    Abstract: In order to accurately determine the residue levels of formaldehyde, acetaldehyde and acetone in water-based adhesives for cigarette, a derivatization-headspace gas chromatography method was developed by optimizing headspace sampling conditions and GC parameters. The adhesive samples were extracted with pure water under oscillation at room temperature, then the extract was centrifuged. The upper solution was placed in a headspace vial, then added PFBHA solution and sealed immediately. The samples were mixed and heated at 70℃ for 50 min in the headspace sampler, then separated on an HP-5 column and determined by flame ionization detector and quantified by external standard method. The results showed that:1) The limits of detection and quantitation for formaldehyde, acetaldehyde and acetone were 0.013-0.023 and 0.042-0.075 mg/kg, respectively. The recoveries were in the range of 95.3%-106.0% with the relative standard deviations(RSDs) no more than 6.1%. 2)The method was applied to the analysis of formaldehyde, acetaldehyde and acetone in water-based adhesives, the test results well agreed with those obtained by a tobacco industrial standard method based on HPLC. The developed method is simple, accurate, environmentally friendly and suitable for the routine determination of formaldehyde, acetaldehyde and acetone in water-based adhesives for cigarette.

     

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