Ruiz-Jiménez Jose, Luque de Castro Maria D
Department of Analytical Chemistry, Annex Marie Curie Building, University of Córdoba, Córdoba, Spain.
Electrophoresis. 2005 Jun;26(11):2231-8. doi: 10.1002/elps.200410398.
Pervaporation has been coupled on-line to capillary electrophoresis (CE) by a simple interface consisting of a modified CE vial. The approach allows volatile analytes to be removed and injected into the capillary meanwhile the sample matrix remains in the pervaporator. By this approach volatile acidity and free sulfur dioxide have been simultaneously determined in wines. The detection limits (LODs) are 1.25 and 5.00 microg/mL, the quantification limits 4.12 and 16.50 microg/mL, and the linear dynamic ranges between LOD and 50 microg/mL and between 0.1 and 0.9 g/L for free sulfur dioxide and volatile acidity, respectively. The repeatability and within laboratory reproducibility, expressed as relative standard deviation (RSD), are 1.61% and 3.00% for free sulfur, and 3.35% and 4.58% for volatile acidity, respectively. The optimal pervaporation time and the time necessary for the individual separation-detection of the target analytes are 6 and 5 min, respectively. The analysis frequency is 7 h(-1) and the sample amount necessary is less than 7 mL. The proposed method and official methods for the analytes were applied to 32 wine samples. A two-tailed t-test was used to compare the methods, which yielded similar results. The errors, expressed as RSD for the two parameters, ranged between 1.3 and 4.1%.
渗透汽化已通过一个由改良的毛细管电泳(CE)小瓶组成的简单接口与毛细管电泳在线联用。该方法能在去除挥发性分析物并将其注入毛细管的同时,使样品基质保留在渗透汽化器中。通过这种方法,已同时测定了葡萄酒中的挥发性酸度和游离二氧化硫。检测限(LOD)分别为1.25和5.00微克/毫升,定量限分别为4.12和16.50微克/毫升,游离二氧化硫和挥发性酸度在LOD与50微克/毫升之间以及0.1至0.9克/升之间的线性动态范围分别为。游离二氧化硫的重复性和实验室内再现性,以相对标准偏差(RSD)表示,分别为1.61%和3.00%,挥发性酸度分别为3.35%和4.58%。目标分析物的最佳渗透汽化时间和单独分离检测所需时间分别为6分钟和5分钟。分析频率为7小时-1,所需样品量小于7毫升。将所提出的方法和分析物的官方方法应用于32个葡萄酒样品。采用双尾t检验比较这些方法,结果相似。以两个参数的RSD表示的误差在1.3%至4.1%之间。