五种磺酰脲类除草剂分离检测方法的建立及其在土壤样品中的应用

Separation of Five Sulfonylurea Herbicides and Application in Soil Sample

研究了高效液相色谱法同时分离测定烟嘧磺隆、甲磺隆、苯磺隆、苄嘧磺隆和吡嘧磺隆等5种不同磺酰脲类除草剂的色谱条件。流动相A为V（乙腈）∶V（水）＝20∶80，流动相B为V（乙腈）∶V（水）＝80∶20，以0．01％磷酸调pH，比较了3种不同的梯度洗脱条件的分离效果。结果表明：梯度3分离效果最佳，流速为0．8 mL/min，检测波长λ＝241 nm，柱温为30℃，5种磺酰脲在18 min达到了基线分离。浓度与峰面积呈良好的线性关系（ R2＝0．9982～0．9998），对标样的检测限在0．02～0．09μg/mL。应用此方法测定加标土壤样品中5种磺酰脲类除草剂的残留量，添加量在3．5 mg/kg时的回收率在89．1％～98．6％。

A high-performance liquid chromatography （ HPLC） method for separation and determination of nicosulfuron,metsulfuron-methyl,tribenuron-methyl,bensulfuron-methyl and pyrazosulfuron-ethyl was studied.The mixture of （A） acetonitrile-water containing 0.01%phosphoric acid （20 ∶80,V/V） and （B） acetonitrile-water （80∶20,V/V） were used as the mobile phase;the effects of three gradient elution proce-dures were compared .The results showed that gradient 3 had the best separation effect .The flow rate was 0.8 mL/min,the detection wavelength was 241 nm,the column temperature was 30 ℃,the baseline sparation was obtained for the five different sulfonylurea herbicides at 18 min.The concentration and peak area showed a good linear relationship （ R2=0.998 2-0.999 8） ,the limits of detection ranged from 0.02-0.07 μg/mL.When this method was used to determine the residues of the five sulfonylurea herbicides in the soil sample ,the recoveries ranged from 89.09%to 98.62 %when 3.5μg/mL standard solution was spiked .