Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah, Iran.
J Sep Sci. 2012 Mar;35(5-6):695-701. doi: 10.1002/jssc.201100836.
Highly porous polyaniline/hexagonally ordered silica sorbent was used for fabrication of the inside needle capillary adsorption trap (INCAT) device. Polyaniline/SBA-15 nanocomposite was synthesized via chemical polymerization technique. The fabricated INCAT device was evaluated to the extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample solutions in combination with gas chromatography (GC)-mass spectrometry (MS). A one at-the-time optimization strategy was applied for optimizing the important extraction parameters such as extraction temperature, extraction time, ionic strength, sampling flow rate, desorption time, and desorption temperature. In optimum conditions (extraction temperature 55 °C, extraction time 20 min, ionic strength 20% (w/v), flow rate 4.5 mL min(-1), desorption temperature 270 °C, desorption time 3 min) the repeatability for one INCAT device (n = 4), expressed as relative standard deviation, was between 4.2 and 10.2% for the tested compounds. The quantitation limits for the studied compounds were between 1 and 5 pg mL(-1). The developed method was successfully applied to spring water sample which was spiked with PAHs with the relative recovery percentages of 87.3-109.1%. The developed method offers the advantage of being simple to use, with shorter analysis times, lower cost of equipment, and thermal stability.
高度多孔聚苯胺/六方有序硅吸附剂被用于制备内针毛细管吸附阱（INCAT）装置。聚苯胺/SBA-15 纳米复合材料是通过化学聚合技术合成的。制备的 INCAT 装置用于从水样中提取一些多环芳烃（PAHs），并与气相色谱（GC）-质谱（MS）联用。采用逐个参数优化策略优化了重要的提取参数，如提取温度、提取时间、离子强度、采样流速、解吸时间和解吸温度。在最佳条件下（提取温度 55°C，提取时间 20 分钟，离子强度 20%（w/v），流速 4.5 mL min(-1)，解吸温度 270°C，解吸时间 3 分钟），一个 INCAT 装置（n = 4）的重复性表示为相对标准偏差，对于测试的化合物在 4.2%至 10.2%之间。研究化合物的定量限在 1 至 5 pg mL(-1)之间。该方法成功地应用于泉水样品中，PAHs 的相对回收率为 87.3-109.1%。该方法具有操作简单、分析时间短、设备成本低和热稳定性好的优点。
