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  

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

作　　者：伍一红[1,2] 龚道新[1,2] 彭筱[1,2] 谢惠[1,2] 韩宝禄[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]中国环境科学研究院,北京100012

出　　处：《色谱》2011年第11期1098-1102,共5页Chinese Journal of Chromatography

基　　金：农业部农药残留试验项目(No.2010P0025)

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0.999 8。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。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 0.999 8.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.

关 键 词：高效液相色谱法 氯硝柳胺乙醇胺盐 残留分析 水稻 稻田 

分 类 号：O658[理学—分析化学]