Preparation of Phenyl group-functionalized magnetic mesoporous silica microspheres for fast extraction and analysis of acetaldehyde in mainstream cigarette smoke by gas chromatography-mass spectrometry
首发时间:2013-05-07
Abstract:Acetaldehyde is a mainstream cigarette smoke constituent, which has been classified as a main toxic component with cytotoxicity or genetoxicity. Owing to its high volatility and reactivity, it is difficult to measure acetaldehyde in complex real samples. In this work, phenyl group-functionalized magnetic mesoporous microshperes was developed as the solid-phase extraction sorbents for enrichment and analysis of acetaldehyde in mainstream cigarette smoke. At first, the functional magnetic microspheres were synthesized through a facile one-pot co-condensation approach. The prepared nanomaterials possessed abundant silanol groups in the exterior surface and numerous phenyl groups in the interior pore-walls, as well as a large surface area (273.5 m2/g), strong superparamagnetism and uniform mesopores (3.3 nm). Meanwhile, these hybrid nanocomposites showed a high efficiency in the extraction and enrichment of aromatic compounds via π-π interactions. In the proposed method, acetaldehyde in main stream cigarette smoke was collected in water and derivatizated with O-2,3,4,5,6-(penta?uorobenzyl)hydroxylamine. The formed acetaldehyde oximes were separated and enriched by the as-prepared adsorbents and subsequently analyzed using GC-MS. Extraction conditions such as amounts of sorbents, eluting solvent, adsorption and desorption time were investigated and optimized to achieve the best efficiency. Method validations including linearity, recovery, repeatability, and limit of detection were also studied. It was found that the suggested methodology provided low detection limit of 0.04 mg/mL, good recovery of 88%, RSD value 9.4%, and linear range of 0.25 ~ 4 mg/mL (R2 = 0.999). The results indicated that the proposed method based on phenyl-functionalized magnetic mesoporous microspheres was rapid, efficient and convenient for the enrichment and analysis of acetaldehyde in tobacco.
keywords: Analytical chemistry Acetaldehyde Cigarette Gas chromatography-mass spectrometry Phenyl group-functionalized magnetic mesoporous microspheres magnetic solid-phase extraction
点击查看论文中文信息
苯基修饰的磁性介孔硅球的制备及其在卷烟主流烟气中乙醛快速富集和气-质联用分析中的应用
摘要:乙醛是卷烟主流烟气中一种具有较强细胞毒性和遗传毒性的主要成分。由于乙醛的高挥发性和反应性,因此一般难以在复杂的实际样品中测量乙醛含量。本研究合成了一种新型的苯基修饰的磁性介孔硅球作为固相萃取剂,用于分析卷烟主流烟气中乙醛含量。所合成的纳米材料孔道内壁有丰富的苯基,超大比表面积(273.5m2/g),极强的超顺磁性以及均匀的介孔孔径(3.3nm)。同时,这些复合材料通过苯基的π-π相互作用对芳香族化合物有很强的富集效率。在所建立的方法中,卷烟主流烟气中的乙醛用水进行收集,然后用邻-(2,3,4,5,6-全氟苯基)羟基氨对乙醛进行衍生。所形成的乙醛肟用所制备的纳米磁性材料进行萃取和富集,并在洗脱后用气相色谱-质谱联用法(GC-MS)对其进行分析。对各项萃取条件,如萃取剂使用量,洗脱溶剂,萃取和洗脱时间等进行了研究和优化,以达到最佳萃取效率。对所建立的萃取方法进行了方法学验证。结果表明,所建立的方法最低检测线可达0.04mg/mL,回收率(88%)及重现性(RSD 9.4%)良好,线性范围为0.25-4mg/mL(R2=0.999)。以上结果表明,基于苯基修饰的磁性介孔硅球的萃取方法快速、高效、便捷,非常适合于烟草主流烟气中乙醛含量的测定。
论文图表:
引用
No.****
同行评议
勘误表
苯基修饰的磁性介孔硅球的制备及其在卷烟主流烟气中乙醛快速富集和气-质联用分析中的应用
评论
全部评论0/1000