高效液相色谱法同时测定稻田中苄嘧磺隆和苯噻酰草胺残留  

Simultaneous determination of bensulfuron-methyl and mefenacet residues in paddy field using high performance liquid chromatography

作　　者：杨丽华[1,2] 龚道新[1,2] 唐晶[1,2] 罗俊凯[1,2] 丁春霞[1,3] 

机构地区：[1]湖南农业大学资源环境学院,湖南长沙410128 [2]湖南农业大学农业环境保护研究所,湖南长沙410128 [3]湖南农业大学理学院,湖南长沙410128

出　　处：《色谱》2012年第1期71-75,共5页Chinese Journal of Chromatography

基　　金：南宁市专利新产品产业化重大科技专项(编号:201106055D)

摘　　要：建立了同时测定稻田(稻田土壤、水和植株)中苄嘧磺隆和苯噻酰草胺残留量的高效液相色谱(HPLC)分析方法。稻田水样品用二氯甲烷直接萃取;稻田土壤样品用碱性乙腈-二氯甲烷(1∶1,v/v)混合液直接提取;水稻植株样品用碱性二氯甲烷提取后,二氯甲烷提取液经弗罗里硅土柱净化。上述样品溶液采用C18不锈钢色谱柱(150mm×4.6 mm,5μm)分离,流动相为水-甲醇(30∶70,v/v),流速为0.5 mL/min,柱温为30℃,紫外检测波长为238 nm,外标法定量。苄嘧磺隆和苯噻酰草胺在0.05～5.00 mg/L范围内的线性关系均很好(r>0.999 9)。在稻田水、土壤和水稻植株中添加3个水平(0.05,0.10,1.00 mg/kg)的苄嘧磺隆和苯噻酰草胺,两者的回收率均在85.39%～113.33%之间,相对标准偏差为0.91%～10.24%。这表明该方法的灵敏度、准确度和精密度均符合农药残留测定的技术要求。An analytical method of high performance liquid chromatography（HPLC） was established for the simultaneous determination of bensulfuron-methyl and mefenacet residues in paddy field（paddy water,soil and rice plant）.The residues in the paddy water was extracted with methylene chloride,and the soil with alkaline mixed solution of acetonitrile-methylene chloride（1∶1,v/v）.The rice plant was extracted with alkaline methylene chloride which was cleaned up by a Florisil column.The separation was performed on a stainless steel C18 column（150 mm×4.6 mm,5 μm） at 30 ℃ by HPLC with an ultraviolet detector（UVD） at 238 nm,and water-methanol（30∶70,v/v） as the mobile phase at a flow rate of 0.5 mL/min.The quantification was performed by external standard.The calibration curves were linear between the peak area and the concentration in the range of 0.05-5.00 mg/L for bensulfuron-methyl and mefenacet,and the correlation coefficients were more than 0.9999.The average recoveries of the two herbicides spiked in the paddy water,soil and rice plant at the three concentration levels of 0.05,0.10 and 1.00 mg/kg ranged from 85.39% to 113.33% with the relative standard deviations of 0.91%-10.24%.The method is characterized by simplicity,sensitivity and accuracy.

关 键 词：高效液相色谱 苄嘧磺隆 苯噻酰草胺 稻田水 稻田土壤 水稻植株 残留分析 除草剂 

分 类 号：O658[理学—分析化学]