β-环糊精液相色谱固定相拆分和测定梨中烯唑醇对映体含量  

Separation and Determination of Diniconazole Enantiomers in Pear on β-Cyclodextrin-based Stationary Phase by HPLC

作　　者：曹志刚[1] 李来生[1,2] 程彪平[1] 张宏福[1] 曾春[1] 谯婷[1] 

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：《分析测试学报》2016年第1期16-22,共7页Journal of Instrumental Analysis

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

摘　　要：制备了一种单脲基衍生化β-环糊精键合有序介孔SBA-15手性固定相（UCDP）,并将其填充于色谱柱中,以甲醇和水为流动相,成功地拆分了手性农药烯唑醇对映体。考察了流动相组成和温度等因素对手性分离的影响,确定最佳条件为：流动相为甲醇-水（40∶60）,流速0.5 m L/min,柱温25℃,检测波长248nm。在优化分离的基础上,建立了一种高效液相色谱快速测定梨中烯唑醇对映体残留量的新方法。梨样品经乙腈提取,氨基固相萃取柱净化后按上述条件测定。单个烯唑醇对映异构体在0.5~125μg/m L范围内呈良好的线性关系。梨样品中分别添加1.25μg/m L和5.0μg/m L两水平的烯唑醇对映体,测得R-烯唑醇的平均回收率分别为92.0%和94.4%,S-烯唑醇的平均回收率分别为91.2%和92.8%。按3倍于噪音信号推算得到单个烯唑醇的检出限为0.02μg/m L。该环糊精类固定相的自制方法简便,脲键固定相更稳定,制备成本较低。所建立的对映体分析方法快速、准确、重现性好,在梨等果蔬样品中农药对映体残留量检测方面有良好的应用前景。A new mono-ureado fl-cyclodextrin-bond ordered mesoporous SBA- 15 chiral stationary phase（UCDP） was prepared and packed into the column. With common methanol -water as mobile phase, the chiral pesticide diniconazole enantiomers was successfully separated by using UCDP. Effects of mobile phase composition and temperature on the chiral separation were investigated. The optimized chromatographic conditions for dinieonazole enantiomers were as follows： mobile phase： methanol - water （40 ： 60） , flow rate ： 0. 5 mL/min, column temperature ： 25 eC , detection wave- length： 248 nm. Based on the above separation conditions, an HPLC method for the rapid determi- nation of diniconazole enantiomer residues in pear was established. The pear samples were extracted with acetonitrile and purified with amino solid extraction column, and determined on UCDP in the a- bove conditions. The good linear relationships for two enantiomers were observed in the range of 0. 5 - 125 μg/mL. The average recoveries of the analytes in pear samples at two spiked concentration levels of 1.25 μg/mL and 5.0 μg/mL were in the ranges of 92. 0% - 94.4% for R-enantiomer, and 91.2% -92. 8% for S-enantiomer, respectively. According to the signal -to -noise of 3 （S/N = 3） , the detection limits of diniconazole enantiomers were 0. 02 Ixg/mL. The UCDP preparation method is simple, and the stationary phase with urea group is stable. The developed method is rapid, accurate and reproducible, and has a good application prospect in the determination of chiral pesticide resi- dues in fruits and vegetables.

关 键 词：高效液相色谱法 环糊精手性固定相 烯唑醇对映体 手性农药 食品安全 

分 类 号：O657.72[理学—分析化学] F767.2[理学—化学]