建立了基质固相分散萃取（matrix solid phase dispersion, MSPD）-反相高效液相色谱(reversed phase high performance liquid chromatography, RP-HPLC)检测利谷隆、灭草隆、敌草隆和绿麦隆4种苯脲类除草剂的新方法。茶叶样品与C18填料混合碾磨后与中性氧化铝一起装柱,二氯甲烷为淋洗剂,使样品的萃取与净化一步完成。讨论了MSPD法和色谱分析的各种影响因素,最佳实验条件下灭草隆在0.01~10.00 mg/L范围内线性关系良好,检测限为5 μg/L;绿麦隆、敌草隆和利谷隆在0.025~10.00 mg/L范围内线性关系良好,检测限为10 μg/L。4种除草剂在茶叶样品中的回收率在83.5%~100.4%之间,相对标准偏差小于7.1%。该方法简单、快速、干扰少、回收率高,符合茶叶中除草剂残留分析要求。
A new method for the simultaneous determination of 4 herbicides (Monuron, Chlortoluron, Diuron and Linuron) was established with MSPD-RP-HPLC. The mixture of tea samples and C18 stuffing were pulverized, then mixed with alumina packed to a syringe column, the extraction and purification of the samples were carried out with one-step using dichloromethane as eluting reagent. The effecting factors of MSPD and conditions of the chromatography were discussed. Under optimum conditions, the linear ranges of Monuron was 0.01~10.0 mg/L with 5 μg/L of the detection limits, and the linear ranges of Chlortoluron, Diuron and Linuron were 0.025~10.0 mg/L with 10 μg/L of the detection limits. The average recoveries of 4 herbicides ranged from 83.5% to100.4% with less than 7.1% of the relative standard deviations in tea samples. The method suggested was simple, rapid, and less interference with high recovery rate, and meet the analytical requirements of herbicide residues in tea.
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