优化用于气相色谱 - 质谱检测水中三嗪类化合物测定的固相微萃取方法。
Optimisation of a solid-phase microextraction procedure for the determination of triazines in water with gas chromatography-mass spectrometry detection.
作者信息
Frías S, Rodríguez M A, Conde J E, Pérez-Trujillo J P
机构信息
Department of Analytical Chemistry, Nutrition and Food Science, University of La Laguna, Afsco Fco Sanchez, s/n, La Laguna, 38071 Santa Cruz de Tenerife, Spain.
出版信息
J Chromatogr A. 2003 Jul 25;1007(1-2):127-35. doi: 10.1016/s0021-9673(03)00957-9.
A procedure based on solid-phase microextraction (SPME) and gas chromatography-mass spectrometry, operating in the chemical ionisation mode, was developed and optimised in order to determine 10 triazines in water samples. Five different SPME fibers available for analysis [polydimethylsiloxane (PDMS) 100 microm, polyacrylate (PA) 80 microm, PDMS-divinylbenzene (DVB) 65 microm, Carbowax (CW)-DVB 65 microm, and Carboxen (CAR)-PDMS 75 microm] were tested, and PDMS-DVB was selected. To enhance the sensitivity of the SPME, variables affecting adsorption and desorption steps such as temperature, time, pH and ionic strength of the solution were optimised. Detection limits obtained were ranged between 2 and 17 ng l(-1), and precision values were below 8% for the selected PDMS-DVB fiber. The optimised method was applied to real water samples and no triazines were detected.
为测定水样中的10种三嗪，开发并优化了一种基于固相微萃取（SPME）和化学电离模式的气相色谱-质谱联用方法。测试了可用于分析的5种不同的SPME纤维[100μm聚二甲基硅氧烷（PDMS）、80μm聚丙烯酸酯（PA）、65μm PDMS-二乙烯基苯（DVB）、65μm聚乙二醇（CW）-DVB和75μm碳分子筛（CAR）-PDMS]，并选择了PDMS-DVB。为提高SPME的灵敏度，对影响吸附和解吸步骤的变量（如温度、时间、溶液的pH值和离子强度）进行了优化。获得的检测限在2至17 ng l(-1)之间，所选PDMS-DVB纤维的精密度值低于8%。将优化后的方法应用于实际水样，未检测到三嗪。
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