Zhang Xinzhong, Ji Hong, Wang Xuemei, Fan Lin, Liu Jingwei, Zhang Wen, Du Xinzhen, Lu Xiaoquan
Key Laboratory of Water Security and Water Environment Protection in Plateau Intersection, Ministry of Education, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou, 730070, PR China; Lanzhou Institute for Food and Drug Control, Key Laboratory of Pesticide and Veterinary Drug Monitoring for State Market Regulation, Lanzhou, 730050, PR China.
Shengli Township People's Government of Kezuo Middle Banner, Tongliao, 029307, PR China.
Anal Chim Acta. 2024 Aug 22;1318:342926. doi: 10.1016/j.aca.2024.342926. Epub 2024 Jun 29.
Since the severe hazard to the ecosystem and widespread distribution through biological and man-made ways of polycyclic aromatic hydrocarbons (PAHs), it is very urgent to establish the ultrasensitive analytical method to quantitatively and directly monitor PAHs in real samples. However, because of the complicated environmental matrix and their trace concentration, the pre-concentration process is a necessary step to analyze of these compounds. In this study, solid phase microextraction (SPME) technique was proposed to separate and enrich fifteen trace PAHs from environmental samples.
In this work, a honeycomb-like triazine-based conjugated microporous polymers (T-CMPs) were prepared by Yamamoto reaction and firstly used as SPME coating material for the ultrasensitive direct-immersion-SPME of PAHs prior to high performance liquid chromatography-fluorescence detector (HPLC-FLD). The synthesized T-CMPs was characterized using various spectroscopy and electron microscopy techniques. The unique porous network of T-CMPs might deliver abundant adsorption sites for PAHs. Orthogonal experimental design (OED) was used to investigate the influence of four experimental parameters on the enrichment ability. Under optimal situation, a wide linear range (which lasted from 0.003 to 1000 μg L) with the coefficients of determination (R) varying 0.9981 to 0.9993 was obtained. The limits of detection (LODs) for the analytes varied from 0.001 to 1.650 μg L, and the limits of quantification (LOQs) were between 0.003 and 4.960 μg L. The proposed method was effectively employed to the simultaneous and ultrasensitive detection of fifteen PAHs in industrial wastewaters. The relative recoveries for PAHs analysis varied from 74.6 % to 105 % with the relative standard deviations (RSD) of 0.1 %-7.5 % in real water samples.
The prepared SPME coating material exhibited a simultaneous, high extraction and adsorption capacity for fifteen PAHs due to its honeycomb-like porous structure, ultra-large specific surface area, strong π-π stacking, and hydrophobic interactions. The present research developed a novel strategy for the construction of SPME fiber coating composites and demonstrated great application potential in the field of sample pretreatment and environmental analytical chemistry.
由于多环芳烃(PAHs)对生态系统危害严重且通过生物和人为方式广泛分布,因此建立超灵敏分析方法以定量和直接监测实际样品中的PAHs非常迫切。然而,由于环境基质复杂且其浓度痕量,预浓缩过程是分析这些化合物的必要步骤。在本研究中,提出了固相微萃取(SPME)技术用于从环境样品中分离和富集15种痕量PAHs。
在本工作中,通过山本反应制备了一种蜂窝状三嗪基共轭微孔聚合物(T-CMPs),并首次将其用作高效液相色谱-荧光检测器(HPLC-FLD)之前PAHs超灵敏直接浸入式SPME的涂层材料。使用各种光谱和电子显微镜技术对合成的T-CMPs进行了表征。T-CMPs独特的多孔网络可能为PAHs提供丰富的吸附位点。采用正交实验设计(OED)研究了四个实验参数对富集能力的影响。在最佳条件下,获得了宽线性范围(0.003至1000μg/L),测定系数(R)在0.9981至0.9993之间变化。分析物的检测限(LOD)为0.001至1.650μg/L,定量限(LOQ)在0.003至4.960μg/L之间。所提出的方法有效地用于工业废水中15种PAHs的同时超灵敏检测。在实际水样中,PAHs分析的相对回收率为74.6%至105%,相对标准偏差(RSD)为0.1%-7.5%。
所制备的SPME涂层材料由于其蜂窝状多孔结构、超大比表面积、强π-π堆积和疏水相互作用,对15种PAHs表现出同时、高萃取和吸附能力。本研究开发了一种构建SPME纤维涂层复合材料的新策略,并在样品预处理和环境分析化学领域展示了巨大的应用潜力。