| 熊伟娜,夏婷婷,陈景文,蔡喜运.土壤中苯线磷及其转化产物对映体的同时分析[J].农业环境科学学报,2014,33(4):708-714. |
| 土壤中苯线磷及其转化产物对映体的同时分析 |
| Direct Enantioselective Determination of Fenamiphos and Its Two Metabolites in Soils Using QuEChERS-HPLC |
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| DOI：10.11654/jaes.2014.04.013 |
| 中文关键词: 对映体拆分 苯线磷 转化产物 QuEChERS 土壤 |
| 英文关键词: enantioseparation fenamiphos transformation products QuEChERS soil |
| 基金项目: |
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| 摘要点击次数: 2013 |
| 全文下载次数: 1955 |
| 中文摘要: |
| 采用QuEChERS预处理技术，结合高效液相色谱拆分，建立了土壤中苯线磷及其转化产物对映体的同时分析方法。苯线磷及其转化产物亚砜和砜单独易于实现手性拆分，但三者手性拆分机制不同（依赖于流动相组成和温度），常规色谱参数优化难以实现它们的同时手性分离。通过向流动相 （87%正己烷/13%异丙醇， V/V）中加入微量水（0.02%），实现了三种化合物对映体的基线分离。联合QuEChERS前处理技术，在该色谱条件下，苯线磷及其转化产物各对映体在土壤中[0.05（0.1）、0.5、5 mg·kg-1三个添加水平]的加标回收率和相对标准偏差分别为82.5%~97.4%和2.5%~6.1%，表明该方法可在对映体水平上直接分析土壤样品中的苯线磷及其转化产物。研究结果将为苯线磷的环境转化过程及残留风险评估研究提供测试技术。 |
| 英文摘要: |
| Direct determination of enantiomers of fenamiphos and its major transformation products（i.e., sulfoxide and sulfone） was achieved using a combination of chiral high performance liquid chromatography（HPLC） and modified QuEChERS（Quick, Easy, Cheap, Effective, Rugged and Safe） preprocessing technique. These compounds were separated individually on a HPLC system equipped with a Chiralpak AD-H stationary phase, via distinct chiral resolution mechanisms depending on organic alcohols and temperature. It was difficult to achieve direct chiral resolution of a mixture of these compounds under general conditions. Here, trace water 0.02% was added as a modifier to the mobile phase comprising n-hexane and 2-propanol（87/13, V/V）, yielding baseline separation of the mixture. This method, in combination with modified QuEChERS technique, was applied to determine these compounds in soil samples spiked at the levels of 0.05/0.1, 0.5 and 5 mg·kg-1. The recoveries ranged from 82.5% to 97.4% with relative standard deviations（RSD） of 2.5%~6.1%, validating its application in determination of fenamiphaos residues in soils. |
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