Guan Wenna, Xu Feng, Liu Wenmin, Zhao Jinghong, Guan Yafeng
Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China.
J Chromatogr A. 2007 Apr 13;1147(1):59-65. doi: 10.1016/j.chroma.2007.01.132. Epub 2007 Feb 4.
A novel polar solid-phase microextraction (SPME) fiber coated with poly(phthalazine ether sulfone ketone) (PPESK) was prepared by immersion precipitation technique. The microstructure of the coating exhibits a sponge-like sublayer supporting a dense cracking shaped top layer (about 1 microm in thickness). This coating shows long lifetime (up to 100 times) and is stable at desorption temperature up to 290 degrees C due to the rigid aromatic rings in chemical structure. We evaluated the extraction-desorption properties of the PPESK fiber for nitroaromatic explosives in aqueous samples. The parameters affecting the extraction were optimized, including extraction temperature and time, salt addition, desorption temperature and time. Limits of detection (LOD), precisions and linear dynamic range for the analysis of explosives by SPME-GC/TSD or ECD were evaluated. Limits of detection of the new fiber was three orders of magnitude lower than those with carbowax/divinylbenzene (CW/DVB), and the relative standard deviation (RSD) of single fiber and fiber-to-fiber were less than 9.3 and 10.4%, respectively. The results demonstrated that the PPESK coating exhibited high extraction efficiency for nitroaromatic compounds due to the pi-pi interaction, dipole-dipole interactions and interactions by polar functional groups. The method was applied to the analysis of nitroaromatic explosives in real aqueous samples including seawater and groundwater samples, with relative recoveries better than 90.7%.
采用浸没沉淀技术制备了一种新型的涂覆有聚(酞嗪醚砜酮)(PPESK)的极性固相微萃取(SPME)纤维。涂层的微观结构呈现出一个海绵状的底层,支撑着一个致密的裂纹状顶层(厚度约为1微米)。由于化学结构中的刚性芳环,这种涂层具有较长的使用寿命(高达100次),并且在高达290℃的解吸温度下稳定。我们评估了PPESK纤维对水样品中硝基芳香族炸药的萃取-解吸性能。优化了影响萃取的参数,包括萃取温度和时间、加盐量、解吸温度和解吸时间。评估了通过SPME-GC/TSD或ECD分析炸药的检测限(LOD)、精密度和线性动态范围。新纤维的检测限比聚乙二醇/二乙烯基苯(CW/DVB)纤维低三个数量级,单根纤维和不同纤维之间的相对标准偏差(RSD)分别小于9.3%和10.4%。结果表明,由于π-π相互作用、偶极-偶极相互作用以及极性官能团之间的相互作用,PPESK涂层对硝基芳香族化合物具有较高的萃取效率。该方法应用于海水和地下水等实际水样中硝基芳香族炸药的分析,相对回收率优于90.7%。