Cao Weixin, Yang Biyi, Qi Feifei, Qian Liangliang, Li Jian, Lu Lingeng, Xu Qian
Key Laboratory of Environmental Medicine Engineering, Ministry of Education, School of Public Health, Southeast University, Nanjing 210009, China.
Suzhou Municipal Center for Disease Prevention and Control, Suzhou 215004, China.
J Chromatogr A. 2017 Mar 31;1491:16-26. doi: 10.1016/j.chroma.2017.02.035. Epub 2017 Feb 20.
Carboxyl modified polyacrylonitrile nanofibers mat (COOH-PAN NFsM) was prepared as a novel solid-phase extraction (SPE) adsorbent for the rapid and effective extraction of atrazine (ATZ) and its toxic metabolites deisopropylatrazine (DIA) and deethylatrazine (DEA) from environmental water samples. Without any pre-treatment but only with the simple filter, water samples passed through pre-conditioned COOH-PAN NFsM, which integrated extraction, purification and concentration into one single step, and the eluent was directly analyzed by high performance liquid chromatography-diode array detection (HPLC-DAD). Under the optimized conditions, the target analytes in 10mL of water sample could be completely extracted by only 4mg of COOH-PAN NFsM, and easily eluted using 400μL of methanol, indicating a high efficiency in both adsorption and desorption. Satisfactory linearity was achieved in the range of 0.4-40.0ngmL for DIA, and 0.3-40.0ngmL for DEA and ATZ. The limit of detection (LODs) were 0.12, 0.09 and 0.09ngmL for DIA, DEA and ATZ, respectively. The recoveries ranged from 81.35 to 120.32%, with the intra-day and inter-day relative standard deviations of 4.03-9.81% even after the 6-cycle usage of NFsM. And, using just 10mL loading sample, the LOD had already satisfied the demand of surface water quality monitoring levels, revealing the good sensitivity of the proposed method.
制备了羧基改性聚丙烯腈纳米纤维毡(COOH-PAN NFsM)作为一种新型固相萃取(SPE)吸附剂,用于从环境水样中快速有效地萃取莠去津(ATZ)及其有毒代谢物去异丙基莠去津(DIA)和去乙基莠去津(DEA)。水样无需任何预处理,仅通过简单过滤后流经预先处理过的COOH-PAN NFsM,该过程将萃取、净化和浓缩整合为一步,然后直接用高效液相色谱-二极管阵列检测(HPLC-DAD)分析洗脱液。在优化条件下,仅4mg的COOH-PAN NFsM就能完全萃取10mL水样中的目标分析物,并用400μL甲醇即可轻松洗脱,表明其在吸附和解吸方面均具有高效性。DIA在0.4 - 40.0ng/mL范围内、DEA和ATZ在0.3 - 40.0ng/mL范围内均获得了令人满意的线性关系。DIA、DEA和ATZ的检测限(LOD)分别为0.12、0.09和0.09ng/mL。回收率在81.35%至120.32%之间,即使在NFsM经过6次循环使用后,日内和日间相对标准偏差仍为4.03 - 9.81%。而且,仅使用10mL进样量时,检测限就已满足地表水水质监测水平的要求,表明该方法具有良好的灵敏度。