Pan Jiongxiu, Li Shuming, Dang Fuquan, Zhang Zhiqi, Zhang Jing
Key Laboratory of Analytical Chemistry for Life Science of Shaanxi Province, School of Chemistry & Chemical Engineering, Shaanxi Normal University Xi'an 710062 China
RSC Adv. 2018 Jun 19;8(40):22422-22428. doi: 10.1039/c8ra04394a.
A novel solid-phase microextraction fiber coated with a porous β-cyclodextrin polymer was developed. The porous β-cyclodextrin polymer cross-linked using tetrafluoroterephthalonitrile, possessed well-distributed pores and the largest surface area among current β-cyclodextrin polymers. Scanning electron microscopy revealed that the coating had a continuous wrinkled and folded structure, which guarantees a sufficient loading capacity for contaminants. The properties of the developed fiber were evaluated using headspace solid-phase microextraction of five contaminants as model analytes coupled with gas chromatography-mass spectrometry. Owing to the advantages of a large surface area and three-dimensional cavities, the novel fiber exhibited excellent operational stability and extraction ability. After optimisation of the extraction conditions, including extraction temperature, extraction time, salt effect, and desorption time, validation of the method with water samples achieved good linearity over a wide range (0.01-120 μg L) and low detection limits (0.003-1.600 μg L). The single-fiber and fiber-to-fiber repeatabilities were 1.7-11.0% and 1.9-11.0%, respectively. The method was applied to the simultaneous analysis of five analytes with satisfactory recoveries (76.6-106.0% for pond water and 89.0-105.9% for rainwater).
研制了一种新型的涂覆有多孔β-环糊精聚合物的固相微萃取纤维。使用四氟对苯二甲腈交联的多孔β-环糊精聚合物具有分布均匀的孔隙,并且在目前的β-环糊精聚合物中具有最大的表面积。扫描电子显微镜显示,涂层具有连续的皱纹和折叠结构,这保证了对污染物有足够的负载能力。以五种污染物作为模型分析物,采用顶空固相微萃取结合气相色谱-质谱联用技术对所研制纤维的性能进行了评价。由于具有大表面积和三维空腔的优势,这种新型纤维表现出优异的操作稳定性和萃取能力。在优化了萃取温度、萃取时间、盐效应和解吸时间等萃取条件后,对水样进行方法验证,结果表明在较宽的范围内(0.01 - 120 μg/L)具有良好的线性关系,检测限较低(0.003 - 1.600 μg/L)。单纤维重复性和纤维间重复性分别为1.7 - 11.0%和1.9 - 11.0%。该方法应用于同时分析五种分析物,回收率令人满意(池塘水的回收率为76.6 - 106.0%,雨水的回收率为89.0 - 105.9%)。