Molina M, Silva M
Department of Analytical Chemistry and Ecology, Faculty of Sciences, University of Córdoba, Spain.
Electrophoresis. 2000 Nov;21(17):3625-33. doi: 10.1002/1522-2683(200011)21:17<3625::AID-ELPS3625>3.0.CO;2-K.
A rapid, reliable method for the multiresidue analysis of eight commonly used fungicides by micellar electrokinetic chromatography (MEKC) was developed. Excellent separation of the eight fungicides (carbendazim, metalaxyl, captan, procymidone, folpet, captafol, vinclozolin and iprodione) is achieved within about 10 min by using optimized electrophoretic conditions that include the addition of a mixture of organic modifiers to the running buffer for improved resolution. The sensitivity of the method is enhanced by using an enrichment step that involves on-column high-salt stacking. Limits of detection in the microgram-per-liter region and relative standard deviations from 2.1 to 5.9% are thus obtained for the fungicides without detracting from peak resolution. These results reveal that the high-salt stacking method provides highly improved sensitivity and enables highly flexible adjustment of the selectivity of the separation method. Also, the method surpasses other stacking alternatives used in MEKC and affords routine analyses of fruit juice containing fungicides at trace levels following a straightforward sample treatment. The robustness of the high-salt stacking method as demonstrated in this work makes MEKC methods involving stacking procedures an attractive choice for routine analyses.
建立了一种通过胶束电动色谱法(MEKC)对八种常用杀菌剂进行多残留分析的快速、可靠方法。通过使用优化的电泳条件,包括在运行缓冲液中添加有机改性剂混合物以提高分离度,在约10分钟内实现了八种杀菌剂(多菌灵、甲霜灵、克菌丹、腐霉利、福美双、敌菌丹、乙烯菌核利和异菌脲)的出色分离。该方法的灵敏度通过采用柱上高盐堆积的富集步骤得以提高。因此,在不影响峰分辨率的情况下,获得了微克每升级别的检测限以及2.1%至5.9%的相对标准偏差。这些结果表明,高盐堆积方法提供了显著提高的灵敏度,并能够高度灵活地调整分离方法的选择性。此外,该方法优于MEKC中使用的其他堆积方法,并且在经过简单的样品处理后,能够对含有痕量杀菌剂的果汁进行常规分析。本研究中所展示的高盐堆积方法的稳健性使得涉及堆积程序的MEKC方法成为常规分析的有吸引力的选择。