色谱

色谱 ›› 2012, Vol. 30 ›› Issue (01): 71-75.DOI: 10.3724/SP.J.1123.2011.09021

• 研究论文 • 上一篇    下一篇

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

杨丽华1,2, 龚道新1,2*, 唐晶1,2, 罗俊凯1,2, 丁春霞1,3   

  1. 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
  • 收稿日期:2011-09-16 修回日期:2011-10-31 出版日期:2012-01-28 发布日期:2012-03-01
  • 通讯作者: 龚道新,博士,教授,博士生导师,主要从事农药残留分析及其生态毒理与环境行为等研究. Tel: (0731)84617710,
  • 基金资助:

    南宁市专利新产品产业化重大科技专项(编号: 201106055D).

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

YANG Lihua1,2, GONG Daoxin1,2*, TANG Jing1,2, LUO Junkai1,2, DING Chunxia1,3   

  1. 1. College of Resource and Environment, Hunan Agricultural University, Changsha 410128, China; 2. Institute of Agricultural Environmental Protection, Hunan Agricultural University, Changsha 410128, China; 3. College of Science, Hunan Agricultural University, Changsha 410128, China
  • Received:2011-09-16 Revised:2011-10-31 Online:2012-01-28 Published:2012-03-01

PDF

371

被引次数

20

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(150 mm×4.6 mm, 5 μm)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＞0.9999)。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。

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

Abstract: 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 0.9999. 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.

Key words: bensulfuron-methyl, herbicides, mefenacet, paddy soil, paddy water, residue analysis, rice plants, high performance liquid chromatography (HPLC)