The chiral resolution of pesticides on amylose-tris(3,5-dimethylphenylcarbamate) CSP by HPLC and the enantiomeric identification by circular dichroism
The chiral resolution of pesticides on amylose-tris(3,5-dimethylphenylcarbamate) CSP by HPLC and the enantiomeric identification by circular dichroism
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DOI：
10.1002/chir.20486
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发表时间：
2008-01-01
期刊：
影响因子：
2
通讯作者：
Zhou, Zhiqiang
中科院分区：
文献类型：
--
作者：
Wang, Peng;Liu, Donghui;Zhou, Zhiqiang
合成了直链淀粉-三（3,5-二甲基苯基氨基甲酸酯）（ADMPC），并将其包被在-氨基丙基二氧化硅上制备了手性固定相（CSP）。采用高效液相色谱法在CSP上手性拆分了农药对映体（非诺沙丙乙酯、奎瑟洛福乙酯、乳芬酯、甲甲酰基、苯甲酰基、己噻唑和氟氧基甲基基）。流动相为正己烷-异丙醇，流速为1.0 ml/min。考察了流动相中异丙醇含量和温度对分离度的影响。在优化条件下，对映体除甲酰基部分分辨外，其余对映体均能获得完全分辨。降低异丙醇的含量，提高了保留率和分辨率。温度是优化的重要色谱参数，结果表明，低温并不总是对分辨率有利。对映体采用圆形二色性（CD）检测器进行鉴定，该检测器可提供CD信号[（+）或（-）]，并通过在线扫描获得了在220 ~ 420 nm范围内的CD光谱。
Amylose-tris(3,5-dimethylphenylcarbamate) (ADMPC) was synthesized and coated on gamma-aminopropylsilica to prepare a chiral stationary phase (CSP). The chiral resolutions of seven pesticide enantiomers including fenoxaprop-ethyl, quizalofop-ethyl, lactofen, metalaxyl, benalaxyl, hexythiazox and fluroxypyr-meptyl on the CSP by high-performance liquid chromatography were performed. Mobile phase was n-hexane and isopropanol with a flow rate of 1.0 ml/min. The influences of isopropanol content in the mobile phase and temperature on the resolutions were investigated. Under the optimized conditions the enantiomers could obtain complete resolutions except that metalaxyl got partial resolution. Decreasing the content of isopropanol increased the retention and the resolutions. Temperature was an important chromatographic parameter for optimization, and the results showed that low temperature was not always good to the resolutions. The enantiomers were identified by a circular dichroism (CD) detector which could provide the CD signals [(+) or (-)] and the CD spectra in the range of 220-420 nm by online scanning.