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[方法]对映体分离是研究手性农药在环境中的选择性行为的重要前提之一,而高效液相色谱法是目前应用最为普遍的对映体分离和制备方法。对高效氯氟氰菊酯在纤维素-三-(3,5-二甲基苯基氨基甲酸酯)(Chiralcel OD-H)手性柱上的分离进行了研究,考察了流动相组成、流速以及柱温对分离效果的影响,并对高效氯氟氰菊酯对映体与固定相之间保留和分离的热力学机理进行了讨论。[结果]分别以5种体积比均为15%的醇改性正己烷,分离因子(α)的变化顺序为异丁醇>异丙醇>正丁醇>正丙醇>乙醇;在0.4~1.1 mL/min的流速范围内,分离度(R s)随着流速的增大而逐渐减小;柱温在15~35℃范围内变化时,随着温度的升高分离因子(α)呈降低趋势,两对映体的lnα与1/T呈良好的线性关系,手性拆分过程受焓的控制。[结论]在柱温为25℃,正己烷-异丙醇(体积比90∶10)为流动相,流速1.0 mL/min时,高效氯氟氰菊酯对映体能达到基线分离,分离因子(α)和分离度(Rs)分别为1.55和4.07。
[Method] Enantiomeric separation is one of the most important preconditions to study the selective behavior of chiral pesticides in the environment. However, HPLC is the most widely used enantiomer separation and preparation method. The separation of lambda-cyhalothrin on a chiral column of cellulose-tris- (3,5-dimethylphenylcarbamate) (Chiralcel OD-H) was studied. The effects of mobile phase composition, Flow rate and column temperature on the separation efficiency were discussed. The thermodynamic mechanism of the retention and separation of lambda-cyhalothrin enantiomers and stationary phases was also discussed. [Result] The n-butanol> isopropanol> n-butanol> n-propanol> ethanol were respectively changed in the order of 5% The separation factor (R s) decreased with the increase of the flow rate at a flow rate of 1.1 mL / min. When the column temperature varied from 15 ℃ to 35 ℃, the separation factor (α) increased with the increase of temperature Decreasing the trend, the two enantiomers lnα and 1 / T showed a good linear relationship, chiral resolution process controlled by the enthalpy. [Conclusion] At the column temperature of 25 ℃, n-hexane-isopropanol (volume ratio 90:10) was the mobile phase at the flow rate of 1.0 mL / min, the enantiomeric separation of lambda-cyhalothrin was achieved. α) and resolution (Rs) were 1.55 and 4.07, respectively.