Ruiz-Jiménez J, Luque de Castro M D
Department of Analytical Chemistry, Annex Marie Curie Building, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain.
J Chromatogr A. 2006 Mar 31;1110(1-2):245-53. doi: 10.1016/j.chroma.2006.01.081. Epub 2006 Feb 17.
A fully automated system for solid sample analysis has been developed by on-line coupling a pervaporation module with a capillary electrophoresis system using as interface a flow injection manifold and a modified capillary electrophoresis vial. The pervaporator allows leaching, formation of the volatile analytes and their removal by evaporation and diffusion through a membrane. The isolated analytes are on-line injected into the capillary electrophoresis system meanwhile the solid matrix remains in the pervaporator. By this approach biogenic amines have been determined in fish, meat and sausage. The detection limits (LOD) ranged between 0.2 and 0.6microg/ml, the quantification limits between 0.7 and 1.9microg/ml and the linear dynamic between 0.4 and 400microg/ml. The precision, expressed as relative standard deviation (RSD), ranged between 0.76 and 4.21% for repeatability and between 1.12 and 4.78% for within laboratory reproducibility. The errors, expressed as RSD for all compounds, ranged between 1.64 and 3.42%. The optimal pervaporation time and that necessary for the individual separation/detection of the target analytes are 14 and 12min, respectively. The analysis frequency is higher than 3h(-1) and the sample size 0.1g. A two-tailed t-test, used to compare the proposed method with that based on HPLC, yielded similar results for nine different samples.
通过将渗透蒸发模块与毛细管电泳系统在线耦合,开发了一种用于固体样品分析的全自动系统,该系统使用流动注射歧管和改进的毛细管电泳瓶作为接口。渗透蒸发器允许浸出、挥发性分析物的形成,并通过膜的蒸发和扩散将其去除。分离出的分析物在线注入毛细管电泳系统,而固体基质保留在渗透蒸发器中。通过这种方法,已测定了鱼类、肉类和香肠中的生物胺。检测限(LOD)在0.2至0.6μg/ml之间,定量限在0.7至1.9μg/ml之间,线性动态范围在0.4至400μg/ml之间。以相对标准偏差(RSD)表示的精密度,重复性在0.76%至4.21%之间,实验室内部重现性在1.12%至4.78%之间。以所有化合物的RSD表示的误差在1.64%至3.42%之间。目标分析物的最佳渗透蒸发时间和单独分离/检测所需的时间分别为14分钟和12分钟。分析频率高于3次/小时,样品量为0.1g。用于将所提出的方法与基于HPLC的方法进行比较的双尾t检验,对九个不同样品产生了相似的结果。