色谱

色谱

• 研究论文 • 上一篇    下一篇

高效液相色谱法分析水稻和稻田中的氯硝柳胺乙醇胺盐残留

伍一红1,2, 龚道新1,2*, 彭筱1,2, 谢惠1,2, 韩宝禄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. 中国环境科学研究院, 北京 100012
  • 收稿日期:2011-05-31 修回日期:2011-08-01 出版日期:2011-11-28 发布日期:2011-12-25
  • 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:

    农业部农药残留试验项目(No. 2010P0025)

Determination of niclosamide ethanolamine residue in rice and paddy field by high performance liquid chromatography

WU Yihong1,2, GONG Daoxin1,2*, PENG Xiao1,2, XIE Hui1,2, HAN Baolu1,3   

  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. Chinese Research Academy of Environmental Sciences, Beijing 100012, China
  • Received:2011-05-31 Revised:2011-08-01 Online:2011-11-28 Published:2011-12-25

PDF

601

被引次数

25

摘要： 建立了高效液相色谱(HPLC)测定水稻和稻田中氯硝柳胺乙醇胺盐残留量的分析方法。稻田水和稻秆样品中的氯硝柳胺乙醇胺盐残留用碱性乙酸乙酯直接提取;而稻田土壤、糙米和谷壳样品则先经碱性乙醇提取,再用乙酸乙酯进行萃取。萃取物经弗罗里硅土柱净化后,经Welchrom C18柱分离,采用紫外检测器检测,外标法定量。在0.01～10.00 mg/L范围内,氯硝柳胺乙醇胺盐的峰面积与其质量浓度间呈良好的线性关系,相关系数为0.9998。在稻田水、土壤、稻秆、糙米和谷壳中添加0.01～5.00 mg/kg的氯硝柳胺乙醇胺盐,其平均回收率为93.47%～100.9%,相对标准偏差为1.46%～5.82%,符合农药残留量分析与检测的技术要求。该方法简便、快速,灵敏度高,重现性好,可用于环境系统中氯硝柳胺乙醇胺盐残留量的分析与检测。

关键词: 残留分析, 稻田, 高效液相色谱法, 氯硝柳胺乙醇胺盐, 水稻

Abstract: A high performance liquid chromatographic (HPLC) method was established for the analysis of niclosamide ethanolamine residue in rice and paddy field. The paddy water and plant were extracted with alkaline ethylacetate, while the paddy soil, rice husk and unpolished rice were first extracted with alkaline ethanol, and then with ethylacetate. The extracts were then cleaned-up by a Florisil column and detected by high performance liquid chromatography with an ultraviolet detector (UVD) on a Welchrom C18 column (250 mm×4.6 mm, 5 μm). The calibration curve showed good linearity from 0.01 mg/L to 10.00 mg/L with the correlation coefficient more than 0.9998. The average recoveries of this method were from 93.47% to 100.9% with the relative standard deviations of 1.46%~5.82% at the spiked levels of 0.01~5.00 mg/kg. This method is fast, simple, sensitive, reproducible and practical for the determination of niclosamide ethanolamine residue in paddy fields, and can meet the requirement of the determination of pesticide residues.

Key words: niclosamide ethanolamine, paddy fields, residue analysis, rice, high performance liquid chromatography (HPLC)