Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028, China.
Talanta. 2012 Jan 15;88:222-9. doi: 10.1016/j.talanta.2011.10.036. Epub 2011 Oct 31.
A novel ionic liquid-based pressurized liquid extraction (IL-PLE) procedure coupled with high performance liquid chromatography (HPLC) tandem chemiluminescence (CL) detection capable of quantifying trace amounts of rutin and quercetin in four Chinese medicine plants including Flos sophorae Immaturus, Crateagus pinnatifida Bunge, Hypericum japonicum Thunb and Folium Mori was described in this paper. To avoid environmental pollution and toxicity to the operators, ionic liquids (ILs), 1-alkyl-3-methylimidazolium chloride ([C(n)mim][Cl]) aqueous solutions were used in the PLE procedure as extractants replacing traditional organic solvents. In addition, chemiluminescence detection was utilized for its minimal interference from endogenous components of complex matrix. Parameters affecting extraction and analysis were carefully optimized. Compared with the conventional ultrasonic-assisted extraction (UAE) and heat-reflux extraction (HRE), the optimized method achieved the highest extraction efficiency in the shortest extraction time with the least solvent consumption. The applicability of the proposed method to real sample was confirmed. Under the optimized conditions, good reproducibility of extraction performance was obtained and good linearity was observed with correlation coefficients (r) between 0.9997 and 0.9999. The detection limits of rutin and quercetin (LOD, S/N=3) were 1.1×10(-2)mg/L and 3.8×10(-3)mg/L, respectively. The average recoveries of rutin and quercetin for real samples were 93.7-105% with relative standard deviation (RSD) lower than 5.7%. To the best of our knowledge, this paper is the first contribution to utilize a combination of IL-PLE with chemiluminescence detection. And the experimental results indicated that the proposed method shows a promising prospect in extraction and determination of rutin and quercetin in medicinal plants.
本文描述了一种新型的基于离子液体的加压液体萃取(IL-PLE)与高效液相色谱(HPLC)串联化学发光(CL)检测相结合的方法,可定量分析四种中药(包括槐米、山楂、贯叶连翘和桑叶)中芦丁和槲皮素的痕量。为了避免环境污染和对操作人员的毒性,在 PLE 过程中使用离子液体(ILs),1-烷基-3-甲基咪唑氯化物([C(n)mim] [Cl])水溶液作为萃取剂,取代传统的有机溶剂。此外,化学发光检测因其对复杂基质内源性成分的最小干扰而被利用。仔细优化了影响萃取和分析的参数。与传统的超声辅助萃取(UAE)和热回流萃取(HRE)相比,优化后的方法在最短的萃取时间内,以最少的溶剂消耗,实现了最高的萃取效率。该方法对实际样品的适用性得到了验证。在优化条件下,萃取性能具有良好的重现性,并且观察到良好的线性关系,相关系数(r)在 0.9997 至 0.9999 之间。芦丁和槲皮素的检测限(LOD,S/N=3)分别为 1.1×10(-2)mg/L 和 3.8×10(-3)mg/L。实际样品中芦丁和槲皮素的平均回收率为 93.7-105%,相对标准偏差(RSD)低于 5.7%。据我们所知,这是第一篇将离子液体加压液体萃取与化学发光检测相结合的论文。实验结果表明,该方法在药用植物中芦丁和槲皮素的提取和测定方面具有广阔的前景。