高效液相色谱法测定苹果和西红柿中腈菌唑对映体含量  

Determination of Myclobutanil Enantiomers in Apples and Tomatoes by High Performance Liquid Chromatography

作　　者：张天赐 钟慧 双亚洲 曾庆丽 李良 李来生 ZHANG Tianci;ZHONG Hui;SHUANG Yazhou;ZENG Qingli;LI Liang;LI Laisheng(College of Chemistry,Nanchang University,Nanchang 330047;Center of Analysis and Testing,Nanchang University,Nanchang 330047)

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

出　　处：《分析科学学报》2021年第3期273-278,共6页Journal of Analytical Science

基　　金：国家自然科学基金(No.31860469,21165012);南昌市科技支撑计划(洪科字[2019]258-18号)。

摘　　要：本文建立一种高效液相色谱测定果蔬中腈菌唑对映体残留量的新方法。样品经QuEChERS方法提取,丙基乙二胺和石墨化炭黑吸附剂净化,用磁粒子快速回收处理后,采用自制的含苯甲酰胺键合臂β-环糊精固定相色谱柱,以乙腈-水=12∶88(V/V)作流动相,实现了腈菌唑对映体的完全分离,在221 nm波长下测定苹果和西红柿中腈菌唑对映体含量。结果表明:腈菌唑对映体的线性范围均为0.5~50μg/mL,苹果中两个对映体的平均回收率分别为93.62%和93.34%;西红柿中两个对映体的平均回收率分别为95.43%和94.80%,测定结果的相对标准偏差(RSDs,n=5)为1.27%~2.01%。腈菌唑对映体的最低检出浓度(S/N=3)为0.04μg/mL,实现了β-环糊精类固定相完全拆分腈菌唑。β-环糊精固定相比常用的纤维素类固定相更耐溶剂,适用反相色谱且成本较低,可用于果蔬样品中农药对映体分析检测。A new method for the determination of myclobutanil enantiomer residues in fruits and vegetables by high-performance liquid chromatography was established.Samples were extracted by QuEChERS method,purified by propylethylenediamine adsorbent and graphitized carbon black,and quickly recovered by magnetic particles.The enantiomers of myclobutanil were completely separated by using self-made β-cyclodextrin stationary phase containing benzamide spacer and acetonitrile-water(12∶88,V/V)as mobile phase.The enantiomers of myclobutanil in apples and tomatoes were quantitatively determined at 221 nm.The results showed that the linear ranges of two myclobutanil enantiomers were 0.5-50μg/mL,the average recoveries of the two enantiomers were 93.62% and 93.34% for apples,and 95.43% and 94.80% for tomatoes,respectively,and the RSDs(n=5)were 1.27%-2.01%.The lowest detection concentrations of myclobutanil enantiomers were 0.04μg/mL(S/N=3).Complete resolution of myclobutanil on β-cyclodextrin stationary phase was achieved for the first time.Compared with common cellulose stationary phase,theβ-cyclodextrin-based stationary phase was more solvent-resistant,suitable for reversed-phase chromatography at lower cost,and has application prospect in enantiomer detection of pesticides in fruits and vegetables.

关 键 词：高效液相色谱法 β-环糊精类键合相 腈菌唑对映体 含量测定 果蔬 

分 类 号：O657.7+2[理学—分析化学]