Department of Analytical Chemistry, Faculty of Sciences, Campus A Zapateira, E-15071 A Coruña, Spain.
Talanta. 2010 Mar 15;80(5):2083-92. doi: 10.1016/j.talanta.2009.11.009. Epub 2009 Nov 10.
Simultaneous analysis of 24 carbonyl compounds (alkanals, unsaturated, dicarbonylic and aromatic aldehydes and ketones) derivatized with 2,4-dinitrophenylhydrazine and 16 polycyclic aromatic hydrocarbons (PAHs) using a photodiode-array (PDA) and a fluorescence (FL) detector in series is proposed. The separation is carried out with a reversed-phase column and gradient elution using four solvents (acetonitrile, water, tetrahydrofuran and methanol) in less than 35 min. Several critical pairs of carbonyl compounds with 3 and 4 carbon atoms and different functional groups, isomers of tolualdehyde, aromatic and aliphatic aldehydes were conditional on the gradient elution. Common pre-treatment for two groups of compounds consists in a step of extraction and derivatization in aqueous medium and a further clean-up using a polymeric phase SPE and concentration in a mixture of dichloromethane:methanol. A pre-concentration factor of 50 was achieved by this procedure. Acetone and formaldehyde blanks were minimized and remain controlled with a specific cleaning of glass material and washing the SPE cartridge. The limits of detection (LOD) ranged from 0.006 to 0.18 ng mL(-1) for PAHs and from 2.4 to 10.1 ng mL(-1) for carbonyl compounds and method precision was <or=15% for all analysed compounds. Recoveries were within the range of 95-104% for PAHs except for more volatile compounds (acenaphthene and fluorene) and within the range of 72-113% for carbonyl compounds. The method was applied in water-soluble fraction of PM(10) (atmospheric particulate matter with an aerodynamic diameter less than 10 microm) and the spectral contrast technique was used in the identification of carbonyl compounds.
提出了一种同时分析 24 种羰基化合物（链烷醛、不饱和、二羰基和芳香醛及酮）的方法，这些羰基化合物经 2,4-二硝基苯肼和 16 种多环芳烃（PAHs）衍生后，使用光电二极管阵列（PDA）和荧光（FL）检测器串联进行分析。分离在反相柱上进行，使用四种溶剂（乙腈、水、四氢呋喃和甲醇）进行梯度洗脱，不到 35 分钟即可完成。几个具有 3 和 4 个碳原子和不同官能团的关键羰基化合物对、甲苯醛的异构体、芳香族和脂肪族醛在梯度洗脱条件下是有条件的。两组化合物的共同预处理步骤包括在水介质中进行提取和衍生化，然后使用聚合物固相萃取（SPE）进行进一步净化，并在二氯甲烷：甲醇混合物中浓缩。通过该程序实现了 50 倍的浓缩因子。通过对玻璃材料进行特定的清洁和洗涤 SPE 小柱，最大限度地减少了丙酮和甲醛空白，并对其进行了控制。对于 PAHs，检测限（LOD）范围为 0.006 至 0.18 ng mL(-1)，对于羰基化合物，检测限范围为 2.4 至 10.1 ng mL(-1)，所有分析化合物的方法精密度均<or=15%。对于 PAHs，除了更易挥发的化合物（苊和芴）外，回收率在 95-104%范围内，对于羰基化合物，回收率在 72-113%范围内。该方法应用于 PM(10)（空气动力学直径小于 10 微米的大气颗粒物）水溶性部分，并用光谱对比技术鉴定羰基化合物。
