Hu Yuefang
College of Chemistry and Bioengineering, Hezhou University, Hezhou 542899, Guangxi, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Apr 1;986-987:143-8. doi: 10.1016/j.jchromb.2015.02.016. Epub 2015 Feb 17.
A method of capillary electrophoresis (CE) coupled with electrochemiluminescence (ECL) detection has been applied to detect three major phenylurea herbicides (monuron, monolinuron and diuron) simultaneously. The effects of yam sample preparation, injection voltage and time, detection potential, detection buffer concentration and pH, Ru(bpy)₃(2+) concentration, separation buffer type, separation buffer pH and concentration, separation voltage were investigated in detail. Under optimum conditions, a good baseline separation and highly sensitive detection for monuron, monolinuron and diuron were achieved. The ECL intensity (I) was in proportion to three analytes concentration (ρ) in the range of 0.1-10,000 μg/L for monuron (r≥0.9993), 0.1-18,000 μg/L for monolinuron (r≥0.9995) and 0.1-20,000 μg/L for diuron (r≥0.9997). The detection limits for monuron, monolinuron and diuron were 0.05, 0.04 and 0.01 μg/L (S/N=3), respectively. The developed method was successfully applied for the analysis of monuron, monolinuron and diuron residues in yam simultaneously. The average recoveries are in the ranges of 90.0-99.2% with relative standard deviations less than 3.2%. The limits of detection of the proposed method were 0.010 μg/kg for monuron, 0.008 μg/kg for monolinuron and diuron in yam.
一种毛细管电泳（CE）与电化学发光（ECL）检测联用的方法已被应用于同时检测三种主要的苯脲类除草剂（灭草隆、绿谷隆和敌草隆）。详细研究了山药样品制备、进样电压和时间、检测电位、检测缓冲液浓度和pH值、Ru(bpy)₃(2+)浓度、分离缓冲液类型、分离缓冲液pH值和浓度、分离电压的影响。在最佳条件下，实现了灭草隆、绿谷隆和敌草隆的良好基线分离和高灵敏度检测。对于灭草隆，在0.1 - 10,000 μg/L范围内，电化学发光强度（I）与三种分析物浓度（ρ）成正比（r≥0.9993）；对于绿谷隆，在0.1 - 18,000 μg/L范围内（r≥0.9995）；对于敌草隆，在0.1 - 20,000 μg/L范围内（r≥0.9997）。灭草隆、绿谷隆和敌草隆的检测限分别为0.05、0.04和0.01 μg/L（S/N = 3）。所建立的方法成功应用于同时分析山药中灭草隆、绿谷隆和敌草隆的残留量。平均回收率在90.0 - 99.2%范围内，相对标准偏差小于3.2%。该方法对山药中灭草隆的检测限为0.010 μg/kg，绿谷隆和敌草隆的检测限为0.008 μg/kg。
