Key Laboratory of Chemistry of Northwestern Plant Resources and Key Laboratory for Natural Medicine of Gansu Province, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, PR China.
Talanta. 2010 Aug 15;82(3):1010-6. doi: 10.1016/j.talanta.2010.06.008. Epub 2010 Jun 11.
In this article, a novel method termed as temperature-assisted ionic liquid dispersive liquid-liquid microextraction (TA IL-DLLME) combining high performance liquid chromatography with diode array detection (HPLC-DAD) was developed for the determination of anthraquinones in Radix et Rhizoma Rhei samples. The ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) was used to replace volatile organic solvent as an extraction solvent for the extraction of anthraquinones (aloe-emodin, rhein, emodin, chrysophanol and physcion) from Radix et Rhizoma Rhei. Several important parameters influencing the extraction efficiency of TA IL-DLLME such as the type and volume of extraction solvent and disperser solvent, sample pH, extraction time, extraction temperature, centrifugation time as well as salting-out effects were optimized. Under the optimal conditions, the spiked recovery for each analyte was in the range of 95.2-108.5%. The precisions of the proposed method were varied from 1.1% to 4.4% (RSD). All the analytes exhibited good linearity with correlation coefficients (r(2)) ranging from 0.9986 to 0.9996. The limits of detection for all target analytes were ranged from 0.50 to 2.02 microg L(-1) (S/N=3). The experimental results indicated that the proposed method was successfully applied to the analysis of anthraquinones in Radix et Rhizoma Rhei.
本文提出了一种新的方法,称为温度辅助离子液体分散液液微萃取(TA IL-DLLME),结合高效液相色谱与二极管阵列检测(HPLC-DAD),用于测定大黄药材中的蒽醌类化合物。离子液体(1-己基-3-甲基咪唑六氟磷酸盐)被用作萃取溶剂,以取代挥发性有机溶剂,用于从大黄药材中萃取蒽醌类化合物(芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚)。优化了 TA IL-DLLME 的几个重要参数,如萃取溶剂和分散剂溶剂的类型和体积、样品 pH 值、萃取时间、萃取温度、离心时间以及盐析效应。在最佳条件下,每种分析物的加标回收率在 95.2%-108.5%之间。该方法的精密度变化范围为 1.1%-4.4%(RSD)。所有分析物均表现出良好的线性关系,相关系数(r²)范围为 0.9986-0.9996。所有目标分析物的检测限范围为 0.50-2.02 µg L⁻¹(S/N=3)。实验结果表明,该方法成功应用于大黄中蒽醌类化合物的分析。