Cao Dan-dan, Lü Jian-xia, Liu Jing-fu, Jiang Gui-bin
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085, China.
Anal Chim Acta. 2008 Mar 17;611(1):56-61. doi: 10.1016/j.aca.2008.01.067. Epub 2008 Feb 7.
Nanostructured titania-based solid-phase microextraction (SPME) fibers were fabricated through the in situ oxidation of titanium wires with H(2)O(2) (30%, w/w) at 80 degrees C for 24h. The obtained SPME fibers possess a approximately 1.2microm thick nanostructured coating consisting of approximately 100nm titania walls and 100-200nm pores. The use of these fibers for headspace SPME coupled with gas chromatography with electron capture detection (GC-ECD) resulted in improved analysis of dichlorodiphenyltrichloroethane (DDT) and its degradation products. The presented method to detect DDT and its degradation products has high sensitivity (0.20-0.98ngL(-1)), high precision (relative standard deviation R.S.D.=9.4-16%, n=5), a wide linear range (5-5000ngL(-1)), and good linearity (coefficient of estimation R(2)=0.991-0.998). As the nanostructured titania was in situ formed on the surface of a titanium wire, the coating was uniformly and strongly adhered on the titanium wire. Because of the inherent chemical stability of the titania coating and the mechanical durability of the titanium wire substrate, this new SPME fiber exhibited long life span (over 150 times).
通过在80℃下用H₂O₂（30%，w/w）对钛丝进行原位氧化24小时，制备了基于纳米结构二氧化钛的固相微萃取（SPME）纤维。所获得的SPME纤维具有约1.2μm厚的纳米结构涂层，该涂层由约100nm的二氧化钛壁和100 - 200nm的孔隙组成。将这些纤维用于顶空固相微萃取并结合带有电子捕获检测的气相色谱法（GC - ECD），可改进对二氯二苯三氯乙烷（DDT）及其降解产物的分析。所提出的检测DDT及其降解产物的方法具有高灵敏度（0.20 - 0.98ngL⁻¹）、高精度（相对标准偏差R.S.D. = 9.4 - 16%，n = 5）、宽线性范围（5 - 5000ngL⁻¹）以及良好的线性（估计系数R² = 0.991 - 0.998）。由于纳米结构的二氧化钛是在钛丝表面原位形成的，涂层均匀且牢固地附着在钛丝上。由于二氧化钛涂层固有的化学稳定性以及钛丝基体的机械耐久性，这种新型SPME纤维具有较长的使用寿命（超过150次）。
