Xu Hua-Ling, Li Yan, Jiang Dong-Qing, Yan Xiu-Ping
Research Center for Analytical Sciences, College of Chemistry, Nankai University, 94 Weijin Road, Tianjin 300071, China.
Anal Chem. 2009 Jun 15;81(12):4971-7. doi: 10.1021/ac900743s.
Stainless steel wire has been widely used as the substrate of solid-phase microextraction (SPME) fibers to overcome the shortcomings of conventional silica fibers such as fragility, by many researchers. However, in previous reports various sorbent coatings are always required in conjunction with the stainless steel wire for SPME. In this work, we report the bare stainless steel wire for SPME without the need for any additional coatings taking advantage of its high mechanical and thermal stability. To evaluate the performance of stainless steel wire for SPME, polycyclic aromatic hydrocarbons (PAHs), benzene, toluene, ethylbenzene, chlorobenzene, n-propylbenzene, aniline, phenol, n-hexane, n-octane, n-decane, n-undecane, n-dodecane, chloroform, trichloroethylene, n-octanol, and butanol were tested as analytes. Although the stainless steel wire had almost no extraction capability toward the tested analytes before etching, it did exhibit high affinity to the tested PAHs after etching with hydrofluoric acid. The etched stainless steel wire gave a much bigger enhancement factor (2541-3981) for the PAHs than the other analytes studied (< or = 515). Etching with hydrofluoric acid produced a porous and flower-like structure with Fe(2)O(3), FeF(3), Cr(2)O(3), and CrF(2) on the surface of the stainless steel wire, giving high affinity to the PAHs due to cation-pi interaction. On the basis of the high selectivity of the etched stainless steel wire for PAHs, a new SPME method was developed for gas chromatography with flame ionization detection to determine PAHs with the detection limits of 0.24-0.63 microg L(-1). The precision for six replicate extractions using one SPME fiber ranged from 2.9% to 5.3%. The fiber-to-fiber reproducibility for three parallel prepared fibers was 4.3-8.8%. One etched stainless steel wire can stand over 250 cycles of SPME without significant loss of extraction efficiency. The developed etched stainless steel wire is very stable, highly selective, and reproducible for the SPME of PAHs.
不锈钢丝已被许多研究人员广泛用作固相微萃取(SPME)纤维的基底,以克服传统石英纤维诸如易碎等缺点。然而,在以往的报道中,用于SPME的不锈钢丝总是需要结合各种吸附剂涂层。在本工作中,我们报道了利用不锈钢丝的高机械稳定性和热稳定性,无需任何额外涂层的裸不锈钢丝用于SPME。为了评估不锈钢丝用于SPME的性能,测试了多环芳烃(PAHs)、苯、甲苯、乙苯、氯苯、正丙苯、苯胺、苯酚、正己烷、正辛烷、正癸烷、正十一烷、正十二烷、氯仿、三氯乙烯、正辛醇和丁醇作为分析物。尽管在蚀刻前不锈钢丝对测试分析物几乎没有萃取能力,但在用氢氟酸蚀刻后,它对测试的PAHs表现出高亲和力。蚀刻后的不锈钢丝对PAHs的增强因子(2541 - 3981)比其他研究的分析物(≤515)大得多。用氢氟酸蚀刻在不锈钢丝表面产生了具有Fe(2)O(3)、FeF(3)、Cr(2)O(3)和CrF(2)的多孔且花状结构,由于阳离子-π相互作用而对PAHs具有高亲和力。基于蚀刻后不锈钢丝对PAHs的高选择性,开发了一种用于气相色谱-火焰离子化检测的新SPME方法来测定PAHs,检测限为0.24 - 0.63 μg L(-1)。使用一根SPME纤维进行六次重复萃取的精密度范围为2.9%至5.3%。三根平行制备纤维的纤维间重现性为4.3 - 8.8%。一根蚀刻后的不锈钢丝可以承受超过250次的SPME循环而萃取效率无显著损失。所开发的蚀刻不锈钢丝对于PAHs的SPME非常稳定、高度选择性且可重现。