Chen Yung-Chih, Ao Yi-Ting, Ding Wang-Hsien
Department of Chemistry, National Central University Chung-Li 320 Taiwan
RSC Adv. 2019 Nov 26;9(66):38669-38676. doi: 10.1039/c9ra07544e. eCollection 2019 Nov 25.
Rapid screening of two microcystins (, microcystin-YR (MC-YR) and microcystin-LR (MC-LR)) in surface water samples was performed by a simple and eco-friendly procedure using deep eutectic solvent-based vortex-assisted liquid-liquid microextraction (DES-based VALLME) combined with ultrahigh-performance liquid chromatography and electrospray ionization (+)-quadrupole time-of-flight mass spectrometry (UHPLC-ESI(+)-qTOF-MS) detection. To obtain an efficient water-miscible DES, choline chloride and phenol at a molar ratio of 1 : 2 were used as an extractant for VALLME. To optimize factors of DES-based VALLME, response surface design alongside Box-Behnken design was used. The limits of quantitation (LOQs) were 0.5 ng mL and 0.4 ng mL for MC-YR and MC-LR, respectively, which is sensitive enough to meet the World Health Organization (WHO) maximum guideline level for MC-LR in water of 1.0 ng mL. Moreover, satisfactory precision with relative standard deviations (RSD) for both intra- and inter-day analysis lower than 11%, and trueness (also known as mean extraction recovery) ranged from 85.5 to 113% based on the ICH method validation guideline.
采用基于深共熔溶剂的涡旋辅助液液微萃取（DES 基 VALLME）结合超高效液相色谱和电喷雾电离（+）-四极杆飞行时间质谱（UHPLC-ESI(+)-qTOF-MS）检测的简单且环保的方法，对地表水样品中的两种微囊藻毒素（微囊藻毒素-YR（MC-YR）和微囊藻毒素-LR（MC-LR））进行快速筛查。为获得一种高效的与水混溶的 DES，将摩尔比为 1∶2 的氯化胆碱和苯酚用作 VALLME 的萃取剂。为优化基于 DES 的 VALLME 的因素，采用了响应面设计以及 Box-Behnken 设计。MC-YR 和 MC-LR 的定量限（LOQ）分别为 0.5 ng/mL 和 0.4 ng/mL，该灵敏度足以满足世界卫生组织（WHO）规定的水中 MC-LR 的最大指导水平 1.0 ng/mL。此外，根据 ICH 方法验证指南，日内和日间分析的相对标准偏差（RSD）均低于 11%，精密度良好，真实性（也称为平均萃取回收率）在 85.5%至 113%之间。
