Cháfer-Pericás C, Herráez-Hernández R, Campíns-Falcó P
Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100 Burjassot, Valencia, Spain.
J Chromatogr A. 2006 Sep 1;1125(2):159-71. doi: 10.1016/j.chroma.2006.05.056. Epub 2006 Jun 23.
This paper compares the advantages and disadvantages of two different configurations for the extraction of triazines from water samples: (1) on-fibre solid-phase microextraction (SPME) coupled to conventional liquid chromatography (LC); and (2) in-tube SPME coupled to capillary LC. In-tube SPME has been effected either with a packed column or with an open capillary column. A critical evaluation of the main parameters affecting the performance of each method has been carried out in order to select the most suitable approach according to the requirements of the analysis. In the on-fibre SPME configuration the fibre coating was polydimethylsiloxane (PDMS)-divinylbenzene (DVB). The limits of detection (LODs) obtained with this approach under the optimized extraction and desorption conditions were between 25 and 125 microg/L. The in-tube SPME approach with a C18 packed column (35 mm x 0.5 mm I.D., 5 microm particle size) connected to a switching micro-valve provided the best sensitivity; under such configuration the LODs were between 0.025 and 0.5 microg/L. The in-tube SPME approach with an open capillary column coated with PDMS (30 cm x 0.25 mm I.D., 0.25 microm of thickness coating) connected to the injection valve provided LODs between 0.1 and 0.5 microg/L. In all configurations UV detection at 230 nm was used. Atrazine, simazine, propazine, ametryn, prometryn and terbutryn were selected as model compounds.
(1)纤维上固相微萃取(SPME)与传统液相色谱(LC)联用;(2)管内SPME与毛细管LC联用。管内SPME可通过填充柱或开管毛细管柱实现。为了根据分析要求选择最合适的方法,对影响每种方法性能的主要参数进行了严格评估。在纤维上SPME配置中,纤维涂层为聚二甲基硅氧烷(PDMS)-二乙烯基苯(DVB)。在优化的萃取和解吸条件下,用这种方法获得的检测限(LOD)在25至125μg/L之间。连接切换微型阀的C18填充柱(35mm×0.5mm内径,5μm粒径)的管内SPME方法提供了最佳灵敏度;在这种配置下,LOD在0.025至0.5μg/L之间。连接进样阀的涂有PDMS的开管毛细管柱(30cm×0.25mm内径,0.25μm涂层厚度)的管内SPME方法的LOD在0.1至0.5μg/L之间。在所有配置中,均采用230nm的紫外检测。选择莠去津、西玛津、扑灭通、莠灭净、扑草净和特丁净作为模型化合物。