毛细管电色谱法测定果蔬中粉唑醇对映体的含量  

Determination of flutrifol enantiomers residue in fruits and vegetables by capillary electrochromatography

作　　者：张宏福[1] 李来生[1,2] 曹志刚[1] 曾春[1] 李良[1] 刘琳珍 

机构地区：[1]南昌大学化学学院,江西南昌330031 [2]南昌大学分析测试中心,江西南昌330047

出　　处：《化学研究与应用》2016年第4期544-552,共9页Chemical Research and Application

基　　金：国家自然科学基金项目(21165012)资助;江西省自然科学基金项目(2010GZH0089)资助;江西省教育厅科技项目(GJJ11274)资助

摘　　要：采用原位聚合反应,制备一种磺丁基醚-β-环糊精修饰甲基丙烯酸聚合物毛细管手性电色谱开管柱(SECDP)。采用该电色谱柱,并在流动相中添加少量磺丁基醚β-环糊精,利用固定相和流动相中的磺丁基醚β-环糊精的协同作用,成功地拆分了手性农药粉唑醇对映体。考察了添加剂浓度、pH值、施加电压、温度及有机调节剂的含量对手性分离的影响,初步优化了开管电色谱柱拆分粉唑醇对映体的条件。优化的流动相组成为10 mmol·L^(-1)硼酸钠(pH=9.2),含3.0 mmol·L^(-1)磺丁基醚β-环糊精和体积分数为15%甲醇,施加电压15 kV,温度20℃,压力进样(3 psi×3 s),检测波长204 nm。在上述条件下,粉唑醇对映体分离度可达1.85,分析时间仅为8~12 min。黄瓜、梨、苹果和西红柿果蔬样品用乙腈提取,磁性石墨化碳净化,在上述优化条件下测定果蔬中粉唑醇对映体的残留量。粉唑醇对映体在1.3~250μg·m L^(-1)范围呈良好的线性关系,线性回归方程为:第一个对映体y_1=92.56+176.81x_1,r_1=0.9993;第二个对映体y_2=46.46+177.97x-2,r_2=0.9998。固定相和流动相中带负电荷的磺丁基醚-β-环糊精不仅能提供较强正向电渗流(EOF),同时有较高的手性分离选择性。所发展的开管毛细管电色谱方法是一种操作简单,分离测定快速,溶剂耗量小,测试成本低,环境污染小的方法。A novel sulfobutyl ether β-cyclodextrin chiral open-tubular capillary column（SECDP） for electrochromatgraphy was prepared by methacrylate polymerization in situ. The SECDP column was successfully used for enantioseparation and determination of chiral pesticide flutriafol enantiomers through the synergistic effects of sulfobutyl ether β-cyclodextrin in both the stationary and mobile phases by capillary eletrochromatography（CEC）. Some effect factors,such as chiral additive concentration,pH value,the applied voltage,temperature and organic modifier content on the resolution of flutriafol enantiomers were investigated. The optimized conditions were as follows： a mobile phase was consisting of 10 mmol·L^（-1）sodium borate（pH = 9. 2）,containing 3. 0 mmol·L^（-1）SBE-β-CD and volume fraction 15%methanol,an applied voltage of 15 kV,column temperature at 20℃,pressure injection（3 psi×3 s）,the detection wavelength at 204 nm.The resolution of flutriafol enantiomers reached to 1. 85 within only 8～12 min under the above conditions.The flutriafol from cucumber,pear,apple and tomato samples were extracted with acetonitrile,and purified with magnetic graphitized carbon.The excellent linear relationships were observed in the range of 1. 3～250 μg·m L^（-1）for two flutriafol enantiomers.The regression equations were y_1= 92. 56＋176. 81x_1（r1= 0. 9993） and y_2= 46. 46＋ 177. 97x_2（r_2= 0. 9998）,respectively. The negative sulfobutyl ether β-cyclodextrin in stationary and mobile phases could provide a strong forward electroosmotic flow（EOF） and good separation selectivity.The proposed CEC is a simple,fast and environment-friendly method with less solvent consumption and low cost.

关 键 词：毛细管电色谱法 甲基丙烯酸酯原位聚合物基质 磺丁基醚β-环糊精 手性农药分离 粉唑醇对映体 食品安全分析 

分 类 号：O657.7[理学—分析化学]