抽拔辅助分散固相微萃取技术用于饮料中5种杀菌剂残留检测研究  

Employing syringe-assisted dispersive solid phase microextraction for precision detection of five fungicide residues in beverages

作　　者：康琬琳 张艳超 宋惜木 席雪霏 高海翔[1] 周文峰[1] KANG Wanlin;ZHANG Yanchao;SONG Ximu;XI Xuefei;GAO Haixiang;ZHOU Wenfeng(Department of Applied Chemistry,College of Science,China Agricultural University,Beijing 100193,China)

机构地区：[1]中国农业大学理学院应用化学系,北京100193

出　　处：《农药学学报》2023年第6期1340-1348,共9页Chinese Journal of Pesticide Science

基　　金：国家自然科学基金(21677174,21277172)。

摘　　要：为了快速检测葡萄汁和苹果汁两种果汁,以及绿茶和红茶两种茶饮料样品中嘧菌酯、三唑酮、百菌清、嘧菌环胺和肟菌酯5种杀菌剂的残留,本研究开发了一种绿色、经济易行的抽拔辅助分散固相微萃取方法,通过在β-环糊精/坡缕石上涂覆离子液体,制备了一种新型的萃取材料,并设计了一系列针对目标杀菌剂萃取条件的优化试验,采用液相色谱检测。结果表明:在萃取材料为40 mg、洗脱液丙酮为600μL、进行6次分散循环、7次洗脱循环的条件下,化合物的检出限(LOD)为0.03~0.38μg/L,定量限(LOQ)为0.09~1.15μg/L,富集因子为121~201。对于5种杀菌剂,可检测的线性范围为5~500μg/L,决定系数(R2)在0.9982~0.9999之间,回收率在91%~102%之间。该方法具有较高的精密度和正确度。实际样品测试结果表明,抽拔辅助分散固相微萃取技术可用于饮料中杀菌剂残留的萃取。In this study,a green,economical and easy-to-use syringe-assisted dispersive solid phase microextraction method was developed for the rapid detection of the residues of 5 fungicides(azoxystrobin,triadimefon,chlorothalonil,cyprodinil,trifloxystrobin)in two fruit juices(grape juice and apple juice)as well as two tea drink samples(green tea and black tea).A novel extraction material was prepared by coating ionic liquids onβ-cyclodextrin/attapulgite,and a series of test experiments for the condition optimization of the method were conducted using liquid chromatography for detection.Results revealed that the optimal condition of the method used 40 mg of extraction material and 600μL of acetone for elution,and 6 dispersion cycles and 7 elution cycles were performed.The detection limits(LOD)for the 5 compounds were 0.03-0.38μg/L,and the limits of quantification(LOQ)were 0.09-1.15μg/L,with the enrichment factors ranged from 121 to 201.The linear detection range of the five fungicides was 5 to 500μg/L,with the coefficient of determination(R2)ranging from 0.9982 to 0.9999.The fortified recoveries were 91%-102%.It showed that the method had good precision and accuracy.The testing results for real samples indicated that the syringe-assisted dispersive solid phase microextraction technology can be used for the extraction of residual fungicides in beverages.

关 键 词：抽拔辅助分散固相微萃取 饮料 杀菌剂 残留 离子液体 坡缕石 Β-环糊精 

分 类 号：TS207[轻工技术与工程—食品科学] O657[轻工技术与工程—食品科学与工程]