高效液相色譜法測定水稻及土壤中甲基硫菌靈和多菌靈

劉靜，李明

摘要：建立了一種同時測定甲基硫菌靈和多菌靈在水稻（Oryza sativa L.）及土壤中殘留量的高效液相色譜分析方法。樣品用丙酮與水混合液提取，經(jīng)弗羅里硅土柱凈化后，采用SunFireTM C18色譜柱，甲醇-水（50∶50，V/V）為流動相，流速1.0 mL/min，柱溫30 ℃，進樣量5 μL，在270 nm波長下測定。甲基硫菌靈和多菌靈在0.10～10.00 mg/L間回歸方程分別為：y=1.216 3+4.909 7x、y=3.351 2+8.770 0x，相關系數(shù)分別為0.998 8、0.998 4；水稻中甲基硫菌靈和多菌靈平均回收率分別為79.31%～93.26%、86.87%～95.17%，相對標準偏差分別為3.08%～7.71%、3.49%～7.86%；土壤中甲基硫菌靈和多菌靈平均回收率分別為89.48%～92.60%、96.50%～101.30%，相對標準偏差分別為5.25%～7.72%、4.05%～7.15%。該分析方法簡單、快速、靈敏，具有良好的準確度和精密度，適用于常規(guī)分析。

關鍵詞：水稻（Oryza sativa L.）；土壤；甲基硫菌靈；多菌靈；HPLC

中圖分類號：X592；O657.7+2 文獻標識碼：A 文章編號：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