固相萃取-高效液相色谱法测定粮谷中多种磺酰脲除草剂残留量

SPE-HPLC DETERMINATION OF SULFONYLUREA HERBICIDE RESIDUES IN CEREALS

样品中残留的磺酰脲除草剂,采用SPE-C18和GCB预柱,进行提取和净化,利用适当的洗脱溶剂对固相萃取柱上富集的组分进行选择性淋洗,通过高效液相色谱的紫外检测器进行分析测定,外标法定量;结果:在0.02mg/kg～0.5mg/kg加标范围内,方法的回收率为74.8%～105.3%,相对标准偏差为2.36%～6.33%;可同时检测大米、小麦、大麦、高粱、荞麦等粮谷中的氯磺隆、苯磺隆、苄嘧磺隆、甲磺隆、环胺磺隆、乙基氯嘧磺隆、嘧啶磺隆、吡啶磺隆、苯胺磺隆、烟嘧磺隆、氟嘧磺隆、苯醚磺隆等磺酰脲类除草剂。

One method was build to determine 12 sulfonylurea herbicides in cereals by Solid phase extraction- high performance liquid chromatography. Methods The residues of sulfonylurea herbicides in sample were extracted by acetonitrile and cleaned by SPE （C18 and GCB）. After separated by HPLC, these compounds were detected by UV detection and quantified by external standard. Results The average recoveries in spiked samples ranged from 74.8 % to 105.3 % and relative standard deviations between 2.36 % and 6.33 %. The method could simultaneously determine Chlorsulfuron, Tribenuron- methyl, Bensulfuron-methyl, Metsulfuron- methyl, Cyclosulfuron, Chlorimuron-ethyl, Flazasulfuron, Pyrazosulfuron-ethyl, Ethametsulfuron-methyl, Nicosulfuron, Primisulfuron and Triasulfuron in cereals such as rice, wheat, barley, sorghum, buckwheat,etc. The method is simple, rapid, accurate, sensitive and easy to be promoted and applicated.