Li Jingkun, Li Huijuan, Zhao Yanfang, Wang Shanshan, Chen Xiangfeng, Zhao Ru-Song
Key Laboratory for Applied Technology of Sophisticated Analytical Instruments, Shandong Analysis and Test Centre, Qilu University of Technology (Shandong Academy of Sciences), Shandong, Jinan, People's Republic of China, 250014.
Mikrochim Acta. 2018 Aug 17;185(9):416. doi: 10.1007/s00604-018-2955-7.
A solid-phase microextraction (SPME) fiber coated with a hollow microporous organic network (H-MON) was fabricated for the analysis of short-chain chlorinated paraffins (SCCPs). The sorbent was prepared by reacting tetra(4-ethynylphenyl)methane and 1,4-diiodobenzene using bis-(triphenylphosphine) palladium(II) as the catalyst in the presence of silica sphere templates, which then were removed by hydrofluoric acid. The SCCPs were quantified by GC-MS working in the negative chemical ionization mode. The H-MON has a high specific surface (701 m·g) and microporosity (pore size <2 nm). Extraction temperature, extraction time, and ionic strength of the sample solutions were optimized by using the Box-Behnken design. The head-space SPME exhibits better extraction performance than the direct immersion mode. Under optimal working conditions, the detection limit (3 times of the standard deviation) is 0.03 ng·mL in the water samples. Response is linear in the 0.05-10 ng·mL concentration range. Repeatability and reproducibility, expressed as the relative standard deviations, ranged from 4.6 to 11.0%. The method was successfully applied in the analysis of SCCPs in water, sediments, organisms, and atmospheric particulate matter samples. Graphical abstract Schematic of the fabrication of a hollow microporous organic network (H-MON) on stainless steel fibers for use in SPME. The method was applied to the determination of short-chain chlorinated paraffins in biological, environmental water and atmospheric particulate matter (PM2.5) samples.
制备了一种涂覆有中空微孔有机网络（H-MON）的固相微萃取（SPME）纤维，用于分析短链氯化石蜡（SCCP）。吸附剂是通过在二氧化硅球模板存在下，以双（三苯基膦）钯（II）为催化剂，使四（4-乙炔基苯基）甲烷与1,4-二碘苯反应制备而成，然后用氢氟酸去除模板。采用负化学电离模式的气相色谱-质谱联用仪（GC-MS）对SCCP进行定量分析。H-MON具有高比表面积（701 m²·g）和微孔率（孔径<2 nm）。采用Box-Behnken设计对萃取温度、萃取时间和样品溶液的离子强度进行了优化。顶空固相微萃取比直接浸入模式具有更好的萃取性能。在最佳工作条件下，水样中的检测限（三倍标准偏差）为0.03 ng·mL。在0.05 - 10 ng·mL浓度范围内响应呈线性。以相对标准偏差表示的重复性和再现性范围为4.6%至11.0%。该方法成功应用于水、沉积物、生物体和大气颗粒物样品中SCCP的分析。图形摘要 在不锈钢纤维上制备用于固相微萃取的中空微孔有机网络（H-MON）的示意图。该方法应用于生物、环境水样和大气颗粒物（PM2.5）样品中短链氯化石蜡的测定。
