Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Granada, Spain; Department of Chemistry, Addis Ababa University, Addis Ababa, Ethiopia.
J Sep Sci. 2013 Oct;36(20):3395-401. doi: 10.1002/jssc.201300652. Epub 2013 Sep 1.
A three-phase hollow-fiber liquid-phase microextraction combined with a capillary LC method using diode array detection was proposed for the determination of six sulfonylurea herbicides, triasulfuron, metsulfuron-methyl, chlorsulfuron, flazasulfuron, chlorimuron-ethyl, and primisulfuron-methyl, in environmental water samples. Different factors that can affect the extraction process such as extraction solvent, acidity of the donor phase, composition and pH of the acceptor phase, salt addition, stirring speed, and extraction time were optimized. Under the optimum conditions, detection and quantitation limits between 0.1-1.7 and 0.3-5.7 μg/L, respectively, and enrichment factors ranging from 71 to 548 were obtained. The calibration curves were linear within the range of 0.3-40 μg/L. Intra- and interday RSDs were <6.3 and 8.4%, respectively. The relative recoveries of the spiked ground and river water samples were in the range of 69.4-119.2 and 77.4-111.7%, respectively. The results of the study revealed that the developed methodology involves an efficient sample pretreatment allowing the preconcentration of analytes, combined with the use of a miniaturized separation technique, suitable for the accurate determination of sulfonylurea herbicides in water.
提出了一种三相中空纤维液相微萃取与二极管阵列检测毛细管 LC 法相结合的方法，用于测定环境水样中的六种磺酰脲类除草剂，分别为三唑磺隆、甲磺隆甲酯、氯磺隆、氟唑磺隆、氯嘧磺隆乙酯和吡嘧磺隆甲酯。优化了萃取溶剂、供相酸度、接受相组成和 pH 值、加盐、搅拌速度和萃取时间等影响萃取过程的不同因素。在最佳条件下，检测限和定量限分别为 0.1-1.7 和 0.3-5.7 μg/L，富集因子范围为 71-548。校准曲线在 0.3-40 μg/L 范围内呈线性。日内和日间 RSD 分别小于 6.3%和 8.4%。加标地下水和河水样品的相对回收率分别在 69.4-119.2%和 77.4-111.7%范围内。研究结果表明，所开发的方法涉及一种有效的样品预处理方法，允许对分析物进行预浓缩，结合使用微型化分离技术，适用于水中磺酰脲类除草剂的准确测定。
