Lei Yun, Chen Beibei, You Linna, He Man, Hu Bin
Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan, Hubei, 430072 PR China.
Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan, Hubei, 430072 PR China.
Talanta. 2017 Dec 1;175:158-167. doi: 10.1016/j.talanta.2017.05.040. Epub 2017 May 15.
Polydimethylsiloxane (PDMS)/MIL-100(Fe) coated stir bar was prepared by sol gel technique, and good preparation reproducibility was achieved with relative standard deviations (RSDs) ranging from 2.6% to 7.5% (n=7) and 3.6% to 10.8% (n=7) for bar-to-bar and batch-to-batch, respectively. Compared with commercial PDMS coated stir bar (Gerstel) and PEG coated stir bar (Gerstel), the prepared PDMS/MIL-100(Fe) stir bar showed better extraction efficiency for target triazines compounds. It also exhibited relatively fast extraction/desorption kinetics and long lifespan. Based on it, a method of PDMS/MIL-100(Fe) coated stir bar sorptive extraction (SBSE)-high performance liquid chromatography-ultraviolet detector (HPLC-UV) was developed for the determination of six triazines (simazine, atrazine, prometon, ametryn, prometryne and prebane) in environmental water samples. Several parameters affecting SBSE of six target triazines including extraction time, stirring rate, sample pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.021-0.079μgL. The repeatability RSDs were in the range of 2.3-6.3% (n=7, c=0.5μgL) and the enrichment factors (EFs) ranged from 51.1 to 102-fold (theoretical EF was 200-fold). The proposed method was applied to the analysis of target triazines in environmental water samples, with recoveries of 98.0-118% and 94.0-107% for spiked East Lake water and local pond water samples, respectively.
采用溶胶-凝胶技术制备了聚二甲基硅氧烷（PDMS）/MIL-100（Fe）涂层搅拌棒，棒间和批次间的相对标准偏差（RSD）分别为2.6%至7.5%（n = 7）和3.6%至10.8%（n = 7），制备重现性良好。与市售的PDMS涂层搅拌棒（Gerstel）和PEG涂层搅拌棒（Gerstel）相比，制备的PDMS/MIL-100（Fe）搅拌棒对目标三嗪类化合物具有更好的萃取效率。它还表现出相对较快的萃取/解吸动力学和较长的使用寿命。基于此，建立了一种PDMS/MIL-100（Fe）涂层搅拌棒吸附萃取（SBSE）-高效液相色谱-紫外检测器（HPLC-UV）法，用于测定环境水样中的六种三嗪（西玛津、莠去津、扑灭通、莠灭净、扑草净和草达津）。研究了影响六种目标三嗪SBSE的几个参数，包括萃取时间、搅拌速率、样品pH值、离子强度、解吸溶剂和解吸时间。在最佳实验条件下，检测限（LOD，S/N = 3）在0.021 - 0.079μg/L范围内。重复性RSD在2.3 - 6.3%（n = 7，c = 0.5μg/L）范围内，富集因子（EF）在51.1至102倍之间（理论EF为200倍）。该方法应用于环境水样中目标三嗪的分析，加标东湖水样和当地池塘水样的回收率分别为98.0 - 118%和94.0 - 107%。
