| 胡 杨1#, 习 京1#, 乔子珊1, 张 玥1, 周 挺2, 顾 钢2, 詹家绥1, 陈凤平1*.对比分析不同方法提取土壤中的二氯喹啉酸[J].植物保护,2017,43(4):125-128. |
| 对比分析不同方法提取土壤中的二氯喹啉酸 |
| Comparison of four methods for quinclorac extraction from soil |
| 投稿时间：2017-01-24 修订日期：2017-03-16 |
| DOI： |
| 中文关键词: 二氯喹啉酸 高效液相色谱法 土壤 |
| 英文关键词:quinclorac high performance liquid chromatography soil |
| 基金项目:福建农林大学校杰出青年科研人才计划(xjq201621); 中国烟草总公司福建省公司科技项目(闽烟合同(2014)181号) |
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| 中文摘要: |
| 本文采用4种常用方法分别对福建田土中添加的二氯喹啉酸进行了提取, 并采用高效液相色谱法对其添加回收率进行了测定, 对比分析表明, 当二氯喹啉酸添加浓度为1.25 μg/g时, 方法二即氢氧化钠溶液提取、乙酸乙酯净化法回收率最高, 约为70%, 且杂质峰较小, 基线平稳, 峰形较对称; 重复性高, 两次生物学试验的平均回收率无显著差异, 均略高于70%。方法一即乙腈磷酸水溶液提取、氯化钠净化法, 回收率较高, 但杂质峰较高, 基线不平稳。方法三即硼砂甲醇溶液提取、二氯甲烷净化法, 虽然杂质峰小、基线平稳、峰形较好、但回收率低，约为50%。方法四即甲醇磷酸水溶液直接提取法, 因提取液难以在旋转蒸发仪中浓缩, 因此未继续检测。综合结果表明, 方法二最适用于福建省水稻田二氯喹啉酸的提取。 |
| 英文摘要: |
| Quinclorac was extracted from field soil spiked with quinclorac in Fujian Province by four common methods and the recovery rate was evaluated by high performance liquid chromatography (HPLC). The results showed that the second method was best for Fujian soil when quinclorac was spiked at 1.25 μg/g, in which the quinclorac was extracted with sodium hydroxide solution and purified with ethyl acetate. The second method had the highest recovery rate of about 70%, with small impurity peak, smooth baseline, symmetry shape of target peak and high repeatability. There was no difference between the average recovery rates in the two biological experiments with the second method. High recovery was also obtained when using the first method, in which the quinclorac was extracted with acetonitrile phosphoric acid solution and purified with sodium chloride, while the large impurity peak was presented with unstable baseline. The small impurity peak, smooth baseline, and good shape of target peak appeared when using the third method, in which the quinclorac was extracted with borax methanol solution and purified with dichloromethane, while the recovery was low with the rate of approximate 50%. The fourth method did not proceed because of difficulty in evaporation of the extraction solution in rotary evaporators, in which the quinclorac was extracted using methanol phosphoric acid solution without purification. Taken together, the second method was the most suitable method for quinclorac extraction in paddy field in Fujian Province |
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