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手性拆分和在线心切割二维液相色谱法在蔬菜和水果中三唑类杀菌剂的测定。

Enantioseparation and determination of triazole fungicides in vegetables and fruits by aqueous two-phase extraction coupled with online heart-cutting two-dimensional liquid chromatography.

机构信息

School of Basic Courses, Guangdong Pharmaceutical University, Guangzhou 510006, China.

School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006, China; Thermo Fisher Scientific, Shanghai 201206, China.

出版信息

Food Chem. 2019 Dec 15;301:125265. doi: 10.1016/j.foodchem.2019.125265. Epub 2019 Jul 27.

Abstract

A novel method for determination of triazole fungicides and their enantiomers in foods was developed by aqueous two-phase extraction (ATPE) coupled with two-dimensional liquid chromatography (2D-LC). With an aqueous two-phase system (ATPS) of ethanol/KHPO as biphasic extractant, the effects of the ATPS composition, extraction temperature and time on extraction yields of triazole fungicides were investigated. Optimum conditions were concluded as follows: ethanol concentration 31% (w/w) and KHPO concentration 21% (w/w), extraction temperature 60 °C, extraction time 21 min. Based on reversed-phase separation systems, a 2D-LC was constructed by optimizing chromatographic conditions and online heart-cutting procedures. As a result, eight triazole fungicides and their enantiomers were separated respectively on C18 and cellulose-tris (3,5-dimethylphenylcarbamate) stationary phases, revealing good linear relationship in the range of 0.1218-30.06 μg/mL (R ≥ 0.9984). The detection limits and recoveries were 0.03113-0.3525 μg/mL and 71.57-107.8%, respectively. The ATPE-2D-LC method was successfully applied to chiral analysis of triazole fungicides in fruits and vegetables.

摘要

建立了一种新的通过双水相萃取(aqueous two-phase extraction,ATPE)与二维液相色谱(2D-LC)联用测定食品中三唑类杀菌剂及其对映体的方法。使用乙醇/KHPO 双水相体系(aqueous two-phase system,ATPS)作为两相萃取剂,考察了 ATPS 组成、萃取温度和时间对三唑类杀菌剂萃取效率的影响。优化条件为:乙醇质量分数 31%,KHPO 质量分数 21%,萃取温度 60°C,萃取时间 21min。基于反相分离体系,通过优化色谱条件和在线分段收集程序,构建了二维液相色谱。结果表明,八种三唑类杀菌剂及其对映体在 C18 和纤维素-三(3,5-二甲基苯基氨基甲酸酯)固定相上得到了很好的分离,在 0.1218-30.06μg/mL 范围内具有良好的线性关系(R≥0.9984)。检测限和回收率分别为 0.03113-0.3525μg/mL 和 71.57%-107.8%。该方法成功应用于水果和蔬菜中三唑类杀菌剂的对映体分析。

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