School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenyang 110016, PR China.
Talanta. 2012 Sep 15;99:932-8. doi: 10.1016/j.talanta.2012.07.061. Epub 2012 Aug 1.
A simple and rapid method based on microwave-assisted extraction (MAE) followed by capillary electrophoresis (CE) was developed for the quantification of eight isoquinoline alkaloids in Chelidonium majus L. (Ch. majus). The key parameters affecting CE separation and MAE extraction were investigated and optimized. Complete separation of eight alkaloids was achieved within only 9 min using a 500 mM Tris-H(3)PO(4) buffer (pH 2.5) containing 50% (v/v) methanol and 2mM HP-β-cyclodextrin. The optimal MAE extraction was performed at 60 °C for 5 min with methanol-water-HCl (90:10:0.5, v/v/v) as the extracting solvent, which gave much higher extraction efficiency in significantly shorter time than conventional heat reflux extraction (HRE) and ultrasonic extraction (USE) methods. Good linearities were obtained for all the alkaloids investigated with correlation coefficients above 0.9994. The repeatability and intermediate precision were less than 4.11% and the recoveries ranged from 98.0% to 103.9%. The developed method was successfully applied to 14 Ch. majus samples obtained from different regions of China. Compared with previously reported methods, the present method offers a dramatic savings in overall analysis time and considerable reduction in solvent consumption.
建立了一种基于微波辅助提取（MAE）结合毛细管电泳（CE）的快速分析方法，用于测定白屈菜Chelidonium majus L.（Ch. majus）中的 8 种异喹啉生物碱。考察并优化了影响 CE 分离和 MAE 提取的关键参数。采用 500 mM Tris-H（3）PO（4）缓冲液（pH 2.5），其中含有 50%（v/v）甲醇和 2 mM HP-β-环糊精，仅需 9 min 即可完全分离 8 种生物碱。最佳 MAE 提取条件为甲醇-水-HCl（90:10:0.5，v/v/v），在 60°C 下提取 5 min，与传统热回流提取（HRE）和超声提取（USE）方法相比，该方法提取效率更高，提取时间更短。所有研究的生物碱均具有良好的线性关系，相关系数均大于 0.9994。重复性和中间精密度均小于 4.11%，回收率在 98.0%至 103.9%之间。该方法成功应用于来自中国不同地区的 14 个白屈菜样品。与以前报道的方法相比，本方法大大缩短了总分析时间，显著减少了溶剂消耗。
