Department of Analytical Chemistry, Faculty of Natural Sciences, Comenius University in Bratislava, Mlynska Dolina Bratislava, Slovak Republic.
J Sep Sci. 2012 Mar;35(5-6):674-80. doi: 10.1002/jssc.201100942. Epub 2012 Jan 24.
A new method for the determination of trace glyphosate (GLYP), non-selective pesticide, by CZE with online ITP pre-treatment of drinking waters on a column-coupling (CC) chip has been developed. CC chip was equipped with two injection channels of 0.9 and 9.9 μL volumes, two separation channels of 9.3 μL total volume and a pair of conductivity detectors. A very effective ITP sample clean-up performed in the first channel at low pH (3.2) was introduced for quick CZE resolution and detection of GLYP carried out at higher pH (6.1) in the second channel on the CC chip. The LOD for GLYP was estimated at 2.5 μg/L (15 nmol/L) using a 9.9 |mL volume of the injection channel. ITP-CZE analyses of model and real samples have provided very favorable intra-day (0.1-1.2% RSD) and inter-day (2.9% RSD) repeatabilities of the migration time for GLYP while 0.2-6.9% RSD values were typical for the peak area data. Recoveries of GLYP in spiked drinking water varied in the range of 99-109%. A minimum pre-treatment of drinking water (degassing and dilution) and a short analysis time (ca. 10 min) were distinctive features of ITP-CZE determinations of GLYP on the CC chip with high sample volume loaded, as well.
一种新的方法用于测定痕量草甘膦 (GLYP),非选择性农药,通过 CZE 与在线 ITP 预处理的饮用水在柱耦合 (CC) 芯片已经开发出来。CC 芯片配备了两个注射通道的 0.9 和 9.9 μL 体积,两个分离通道的 9.3 μL 总容积和一对电导率检测器。非常有效的 ITP 样品净化在第一通道在低 pH 值 (3.2) 被介绍了快速 CZE 分辨率和检测 GLYP 在更高的 pH 值 (6.1) 在第二通道的 CC 芯片上进行。LOD 为 GLYP 估计在 2.5 μg/L (15 nmol/L) 使用一个 9.9 |毫升体积的注射通道。ITP-CZE 分析模型和实际样品提供了非常有利的日内 (0.1-1.2% RSD) 和日间 (2.9% RSD) 的重复性迁移时间的 GLYP 而 0.2-6.9% RSD 值是典型的峰面积数据。回收率的 GLYP 在加标饮用水中变化范围为 99-109%。最小的预处理饮用水 (脱气和稀释) 和短的分析时间 (约 10 分钟) 是 ITP-CZE 测定的特点 GLYP 在 CC 芯片上用高体积加载的样品,以及。