高效液相色谱法测定水稻及土壤中甲基硫菌灵和多菌灵
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摘要：建立了一种同时测定甲基硫菌灵和多菌灵在水稻（Oryza sativa L.）及土壤中残留量的高效液相色谱分析方法。样品用丙酮与水混合液提取，经弗罗里硅土柱净化后，采用SunFireTM C18色谱柱，甲醇-水（50∶50，V/V）为流动相，流速1.0 mL/min，柱温30 ℃，进样量5 μL，在270 nm波长下测定。甲基硫菌灵和多菌灵在0.10～10.00 mg/L间回归方程分别为：y=1.216 3+4.909 7x、y=3.351 2+8.770 0x，相关系数分别为0.998 8、0.998 4；水稻中甲基硫菌灵和多菌灵平均回收率分别为79.31%～93.26%、86.87%～95.17%，相对标准偏差分别为3.08%～7.71%、3.49%～7.86%；土壤中甲基硫菌灵和多菌灵平均回收率分别为89.48%～92.60%、96.50%～101.30%，相对标准偏差分别为5.25%～7.72%、4.05%～7.15%。该分析方法简单、快速、灵敏，具有良好的准确度和精密度，适用于常规分析。
关键词：水稻（Oryza sativa L.）；土壤；甲基硫菌灵；多菌灵；HPLC
中图分类号：X592；O657.7+2 文献标识码：A 文章编号：0439-8114（2013）05-1151-03
Analysis of Thiophanate-Methyl and Carbendazim in Rice and Soil by High Performance Liquid Chromatography
LIU Jing，LI Ming
（Institute of Crop Protection， Guizhou University， Guiyang 550025， China）
Abstract： A method for the analysis of thiophanate-methyl and carbendazim residues in rice（Oryza sativa L.） plant and soil was established by high performance liquid chromatography （HPLC）. Samples were ultrasonically extracted with the mixture of acetone and water， purified on the florisil SPE column. The SunFireTM C18 column was used as chromatography column， the mobile phase was the mixture of methanol-water（50∶50， V/V） at a flow rate of 1.0 mL/min， the column temperature was 30 ℃， injection volume was 5.0 μL and detection wavelength was 270 nm. The linear range was 0.10～10.00 mg/L， the regression equations of thiophanate-methyl and carbendazim were y=1.216 3+4.909 7 x and y=3.351 2+8.770 0 x， respectively， coefficient of correlations were 0.998 8 and 0.998 4. The recoveries of thiophanate-methyl and carbendazim were 79.31%～93.26% and 86.87%～95.17%， respectively， relative standard devirations（RSD） were 3.08%～7.71% and 3.49%～7.86% for rice. And the recoveries were 89.48%～92.60% and 96.50%～101.30%， RSD were 5.25%～7.72% and 4.05%～7.15% for soil， respectively. The method could be used for conventional analysis， which was simple， rapid， accurate and sensitive.
Key words： rice（Oryza sativa L.）； soil； thiophanate-methyl； carbendazim； HPLC