高效液相色谱法同时检测稻田中戊唑醇和菌核净(8100字)
摘 要：为了全面准确地评价戊唑醇或菌核净及其相关制剂在稻田中使用后的生态环境安全性，指导该类农药及其相关制剂的科学合理使用；通过添加回收率实验，借助HPLC检测技术，研究并建立了同时检测稻田土壤和水中戊唑醇和菌核净残留量的分析方法。结果表明：①同时检测戊唑醇和菌核净残留量的最佳HPLC条件为：吸收波长为220nm，流动相为甲醇和水的混合液（65:35，v/v），流速采用梯度淋洗法：0～7min: 1.0 mL/min，7～30min:0.5 mL/min。②稻田水样直接采用二氯甲烷萃取，稻田土壤样品则用甲醇-水（7:3）提取，经振荡提取后用二氯甲烷萃取，二氯甲烷萃取液经浓缩后待HPLC检测。③ 当添加浓度为0.05、0.50、1.00 mg/kg时，戊唑醇和菌核净在稻田水中的平均回收率在89.12%～107.21%之间，相对标准偏差（变异系数）在1.25%～8.08%之间；戊唑醇和菌核净在稻田土壤中的平均回收率在80.22%～116.08%之间，相对标准偏差在1.93%～14.05%之间；戊唑醇和菌核净的最小检出量均为：1.0×10-9g，戊唑醇和菌核净在稻田水中的最低检出浓度均为0.05 mg/L，在稻田土壤中的最低检出浓度均为0.05 mg/kg。该检测技术能同时分析和检测稻田水和土壤中戊唑醇和菌核净的残留量，且操作简便、灵敏度和精密度均符合我国农药残留试验准则的技术要求。
关键词：戊唑醇；菌核净；残留量；稻田环境样品；同时检测；HPLC法
Simultaneous Determination of Tebuconazole and Dimetachlone Residues in Paddy Field by High Performance Liquid Chromatography
Abstract: In order to assess the ecological safety both correctly and fully after Tebuconazole and Dimetachlone was used in paddy field.The added recovery experiments and HPLC was applied to establish an analytical method to simultaneously determine the residues of Tebuconazole and Dimetachlone in paddy field. The results showed as follow.
First, the optimum HPLC condition of Simultaneous determination of Tebuconazole and Dimetachlone residues was: absorption wave was 220nm,fluid phase was methanol-water mixture（65:35，v/v）by the step-washing method for velocity (0~7min:1.0 mL/min，7~30min:0.5 ml/min) . Second, the residue of Tebuconazole and Dimetachlone in paddy water was extracted with CH2Cl2,while its residue in paddy soil was extracted by methanol-water mixture(7:3,v/v),after be concentrated ,the extract was re-extracted with CH2Cl2,the re-extract was concentrated,and detected by HPLC. Third, when the added concentration were 0.05,0.50 and 1.00 mg/L,the average recoveries of this two herbicides(Tebuconazole and Dimetachlone) in paddy water ranged from 89.12% to 107.21% with its relative standard deviations between 1.25% and 8.08%,while in paddy soil, it was changed from 80.22% to 116.08% by its relative standard deviations between 1.93% and 14.05%,and the limit of detection of Tebuconazole and Dimetachlone was 1.0×10-9 g, the minimum detectable concentration of this two residues was 0.05 mg/L in paddy water and 0.05 mg/kg in paddy soil . This method could Simultaneously determine and analyse the residue of Tebuconazole and Dimetachlone in both paddy water and soil, it is very characterized with simplicity，sensitivity and accuracy.
Key words: Tebuconazole； Dimetachlone；residue；paddy water and soil；simultaneous determination；HPLC
目 录
摘 要 1
关键词 1
1 前言 2
1.1 戊唑醇和菌核净的简介 2
1.2 戊唑醇和菌核净的研究进展 3
2 研究目的和内容 5
2.1 研究目的 5
2.2 研究内容 5
3 材料与方法 5
3.1 主要仪器设备与试剂 5
3.1.1 主要试剂 5
3.1.2主要仪器设备 5
3.2 HPLC检测条件和提取剂的选择与优化 5
3.2.1 戊唑醇和菌核净检测波长的选择 5
3.2.2 流动相的选择 6
3.2.3 流速的选择与优化 7
3.2.4 提取剂的选择与优化 7
3.3 戊唑醇和菌核净标准工作曲线的绘制 7
3.4 添加回收率实验 8
3.4.1 戊唑醇和菌核净在稻田土壤中的添加回收实验 8
3.4.2 戊唑醇和菌核净在稻田水中的添加回收实验 8
3.4.3 添加回收率的计算公式 8
4 结果与分析 8
4.1 HPLC条件的确定 8
4.2 标准工作曲线 9
4.3方法的准确度与精密度 9
5 结论 11
参考文献 11
致 谢 13
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