摘要
本文建立了低共熔溶剂液相微萃取高效液相色谱法测定5种杀菌剂(三唑醇、嘧霉胺、三唑酮、烯唑醇、嘧菌环胺)的农药残留分析方法,以苯酚作为氢键给体,氯化胆碱作为氢键受体组合而成的低共熔溶剂作为提取溶剂,THF作为分散剂,形成浑浊小液滴,目标分析物被萃取到微量的DESs相中,经过离心,吸取DESs相进高效液相色谱分析。对影响萃取效率的重要因素进行选择和优化。研究表明,氯化胆碱与苯酚在1:2的比率形成的低共熔溶剂萃取效果最好,同时,在最佳的萃取条件(样品容量为5 mL,DES2为150μL,THF为150μL,超声时间为20 min,离心时间为10 min)下进行添加回收率实验,回收率在73.7%~102.3%之间,相对标准偏差(RSD)为0.7%~7.1%,最小检出限(LOD)0.026~0.052μg/L。为实际检测残留农药提供安全可靠的提取和分离技术,减少有机溶剂的使用对环境及人体健康构成的危害。
A method was developed for the determination of five fungicide residues(triadiconazole, pyrimethanil, triadimefon, carbazole, and cyprodinil) by high performance liquid chromatography with deep eutectic solvent as extraction in liquid-phase microextraction. A DES containing phenol as a hydrogen bond donor and choline chloride as a hydrogen bond acceptor was used as the extraction solvent. THF was used as a dispersant solvent to form small droplets of turbidity. The target analyte was extracted into trace DESs phase. After centrifugation, the upper DESs phase was subjected to high-performance liquid chromatography for analysis. Various parameters affecting extraction efficiency were investigated and optimized. The results were shown that the DESa molar ratio of choline chloride and phenol 1:2 is the best extraction efficiency. Under the optimum conditions are as follows: sample volume 5 mL, DES2 150 μL, and THF 150 μL, ultrasonic time 20 min and centrifugation time 10 min. The recoveries were between 73.7%~102.3%, the relative standard deviations(RSDs) were between 0.7%~7.1%, and the low limits of detection(LOD) were 0.026~ 0.052 μg/L.
作者
赵桐桐
张冬昊
郭振福
何扩
王素利
ZHAO Tong-tong;ZHANG Dong-hao;GUO Zhen-fu;HE Kuo;WANG Su-li(Hebei North University Food Safety Research Center, Zhangjiakou 075000, China)
出处
《现代食品科技》
EI
CAS
北大核心
2019年第8期281-286,共6页
Modern Food Science and Technology
基金
河北省自然科学基金项目(B2017405049)
河北省高等学校科学重点研究(ZD2016139)
河北北方学院博士基金项目资助
关键词
低共熔溶剂
液相微萃取
杀菌剂
超高效液相色谱
deep eutectic solvents (DESs)
liquid phase microextraction (LPME)
fungicides
ultra high performance liquid chromatography(UPLC)
