Huang Shang-Da, Huang Hsin-I, Sung Yu-Hsiang
Department of Chemistry, National Tsing Hua University, Hsinchu 30043, Taiwan.
Talanta. 2004 Nov 15;64(4):887-93. doi: 10.1016/j.talanta.2004.03.063.
Solid-phase microextraction (SPME) coupled with high-performance liquid chromatography (HPLC) for the determination of triazine is described. Carbowax/templated resin (CW/TPR, 50mum), polydimethylsiloxane/divinylbenzene (PDMS/DVB, 60mum), polydimethylsiloxane (PDMS, 100mum), and polyacrylate (PA, 85mum) fibers were evaluated for extraction of the triazines. CW/TPR and PDMS/DVB fibers were selected for further study. Several parameters of the extraction and desorption procedure were studied and optimized (such as types of fibers, desorption mode, desorption time, compositions of solvent for desorption, soaking periods and the flow rate during desorption period, extraction time, temperature, pH, and ionic strength of samples). Both CW/TPR and PDMS/DVB fibers are acceptable; a simple calibration-curve method based on simple aqueous standards can be used. The linearity of this method for analyzing standard solution has been investigated over the range 5-1000ngmL(-1) for both PDMS/DVB and CW/TPR fibers. All the correlation coefficients in the range 5-1000ngmL(-1) were better than 0.995 except Simazine and Atratone by CW/TPR fiber. The R.S.D.s range from 4.4% to 8.8 % (PDMS/DVB fiber) and from 2.4% to 7.2% (CW/TPR fiber). Method-detection limits (MDL) are in the range 1.2-2.6 and 2.8-3.4ngmL(-1) for the two fibers. These methods were applied to the determination of trazines in environmental water samples (lake water).
描述了采用固相微萃取（SPME）与高效液相色谱（HPLC）联用测定三嗪的方法。对Carbowax/模板树脂（CW/TPR，50μm）、聚二甲基硅氧烷/二乙烯基苯（PDMS/DVB，60μm）、聚二甲基硅氧烷（PDMS，100μm）和聚丙烯酸酯（PA，85μm）纤维用于萃取三嗪的性能进行了评估。选择CW/TPR和PDMS/DVB纤维作进一步研究。对萃取和解吸过程的几个参数进行了研究和优化（如纤维类型、解吸模式、解吸时间、解吸溶剂组成、浸泡时间和解吸期间的流速、萃取时间、温度、pH值以及样品的离子强度）。CW/TPR和PDMS/DVB纤维均可接受；可采用基于简单水溶液标准的简单校准曲线法。已研究了该方法在5 - 1000ngmL⁻¹范围内分析标准溶液的线性，对于PDMS/DVB和CW/TPR纤维均如此。除了用CW/TPR纤维分析西玛津和莠灭净外，在5 - 1000ngmL⁻¹范围内所有相关系数均优于0.995。相对标准偏差（R.S.D.）范围为4.4%至8.8%（PDMS/DVB纤维）和2.4%至7.2%（CW/TPR纤维）。两种纤维的方法检测限（MDL）范围分别为1.2 - 2.6和2.8 - 3.4ngmL⁻¹。这些方法应用于环境水样（湖水）中三嗪的测定。
