首页> 中文期刊> 《江西农业大学学报》 >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

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

         

摘要

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 .%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%。

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