制备了一种新型的对甲苯脲衍生化β-环糊精键合有序介孔 SBA-15手性固定相（ UCDP），通过红外光谱和元素分析对其结构进行了基本表征。将新固定相用于手性农药粉唑醇对映体的拆分，考察了流动相组成和温度对分离的影响，通过优化分离条件，在反相色谱条件下成功地拆分了粉唑醇对映体。优化的色谱条件为：甲醇-水（40∶60，v／v）为流动相，流速为0.5 mL／min，柱温为25℃，选择205 nm检测波长进行检测。在上述条件下，两对映体的分离度可达1.99，分析时间不超过20 min。在此基础上建立了快速测定香蕉中三唑类手性杀菌剂粉唑醇对映体残留量的新方法，两对映体在0.5～125 mg／L范围均具有良好的线性关系（ r＝0.9997），标准添加法测得粉唑醇对映体的平均回收率为93.4％～101.7％，RSD 为1.07％～2.06％（ n＝4）。按3倍信噪比确定检出限为0.06 mg／L。与常用的涂覆型纤维素固定相相比，新固定相的制备方法简便，制备成本较低。单取代脲键环糊精固定相不仅有稳定的化学结构和色谱性能，而且对粉唑醇对映体显示出较高的分离选择性，所建立的方法可用于快速监测食品中农药对映体残留量，对解决食品中的手性农药安全问题有着重要的研究意义。
A new mono-methyl phenyl ureado β-cyclodextrin-bonded order mesoporous SBA-15 chiral stationary phase( UCDP)was prepared. The basic structure characterization of the new stationary phase was carried out by infrared spectroscopy and elemental analysis. The new packing material was used to separate chiral fungicide flutriafol enantiomers by HPLC. The effects of the composition of mobile phase and column temperature on the enantioseparation of flutriafol were investigated. The flutriafol enantiomers were successfully resolved under the optimized conditions,which were as follows:methanol-water( volume ratio of 40 ∶60 ) as mobile phase at a flow rate of 0. 5 mL/min,the column temperature at 25 ℃,the detection wavelength at 205 nm. The resolution of the two enantiomers was up to 1. 99 within 20 min under the above conditions. Based on the study,a new method for the determination of flutri-afol enantiomers in banana was established. Good linear relationships were observed in the mass concentration range of 0. 5-125 mg/L( r=0. 999 7)for the two enantiomers. The average spiked recoveries were 93. 4%-101. 7% with RSDs of 1. 07%-2. 06%( n=4). The detection limit was 0. 06 mg/L( S/N=3). Compared with the commonly used cellulose stationary phase,the preparation of new stationary phase is simple at low cost. The β-cyclodextrin-bonded stationary phase with mono-methyl phenyl ureado has high chemical stability,reproducible chromato-graphic property and high selectivity for flutriafol enantiomers. The developed analytical method is suitable for the fast monitoring of chiral pesticide residues in foods and has research signifi-cance to solve the food safety problems of chiral chemicals.
参考文献
| [1] | Qiu, J.;Dai, S.;Zheng, C.;Yang, S.;Chai, T.;Bie, M..Enantiomeric separation of triazole fungicides with 3-μm and 5-μml particle chiral columns by reverse-phase high-performance liquid chromatography[J].Chirality: The pharmacological, biological, and chemical consequences of molecular asymmetry,20116(6):479-486. |
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