Key Laboratory of Natural Pesticide and Chemical Biology, Ministry of Agriculture & Key Laboratory of Bio-Pesticide Innovation and Application of Guangdong Province, South China Agricultural University, 483 Wushan Road, Guangzhou, 510642, China.
Sci Rep. 2020 Mar 13;10(1):4709. doi: 10.1038/s41598-020-61755-z.
A simple and effective method for determining five pyrethroid residues in herbal tea by ultrasound-enhanced temperature-controlled (UETC) ionic liquid dispersive liquid-liquid microextraction (IL-DLLME) coupled with high performance liquid chromatography-diode array detection (HPLC-DAD) was developed. The use of ultrasonication and heating improved the ability of the ionic liquid to extract the analytes. Various parameters that affect the extraction efficiency were investigated and optimized using single factor experiments and response surface design. The optimum conditions of the experiment were 121 µL of [HMIM][PF6] (extraction solvent), 794 µL of acetonitrile (dispersive solvent), a heating temperature of 40°C, a sonication time of 3.6 min and a pH of 2.9. Under optimized conditions, the linearity was in the range of 0.05-5 mg L with correlation coefficients above 0.9993. The limits of detection and quantification were 1.25-1.35 µg L and 5 µg L, respectively. The mean recoveries of the five pyrethroids ranged from 74.02% to 109.01%, with RSDs below 9.04%. The proposed method was reliable for the analysis of pyrethroids in Chinese herbal tea.
超声强化控温水相离子液体分散液液微萃取结合高效液相色谱-二极管阵列检测法测定凉茶中五种拟除虫菊酯残留的简便、有效方法。超声和加热增强了离子液体萃取目标物的能力。采用单因素实验和响应面设计法考察并优化了影响萃取效率的各种参数。实验的最佳条件为:[HMIM][PF6](萃取溶剂)121µL,乙腈(分散溶剂)794µL,加热温度 40°C,超声时间 3.6min,pH 值 2.9。在优化条件下,五种拟除虫菊酯的线性范围为 0.05-5mg·L,相关系数均大于 0.9993。检出限和定量限分别为 1.25-1.35µg·L 和 5µg·L。五种拟除虫菊酯的平均回收率为 74.02%-109.01%,相对标准偏差均低于 9.04%。该方法可靠,可用于分析中草药中的拟除虫菊酯。