Liu Lihong, Fan Liuyin, Chen Hongli, Chen Xingguo, Hu Zhide
Department of Chemistry, Lanzhou University, P.R. China.
Electrophoresis. 2005 Aug;26(15):2999-3006. doi: 10.1002/elps.200500069.
A simple, rapid, and accurate method for the separation and determination of physcion, chrysophanol, aloe-emodin, and emodin in Rhubarb, Juemingzi, and Chinese herbal preparations was developed by combination of flow injection-capillary zone electrophoresis for the first time. The analysis was carried out using an unmodified fused-silica capillary (75 mm x 50 microm ID x 375 microm OD, effective separation length of 48 mm) and direct ultraviolet detection at 254 nm. By a series of optimization, the sample solvent consisted of NaOH (100 mmol/L) and ACN (1:1 v/v), and a running buffer composed of 15 mmol/L sodium borate - 12.5 mmol/L sodium dihydrogen phosphate - 42% v/v ACN (pH 10.1) was applied for the separation of the four anthraquinones. The separation was rapid and highly reproducible, with complete resolution of all four compounds within 6 min. The sample throughput rate could reach up to 12 per h. The repeatability (defined as relative standard deviation) was 4.45, 4.44, 4.34, 0.61% with peak height evaluation and 1.62, 0.89, 2.49, 2.19% with peak area evaluation for physcion, chrysophanol, aloe-emodin, and emodin, respectively.
首次通过流动注射-毛细管区带电泳联用技术开发了一种简单、快速且准确的方法,用于分离和测定大黄、决明子及中草药制剂中的大黄素甲醚、大黄酚、芦荟大黄素和大黄素。分析采用未修饰的熔融石英毛细管(75 mm×50 μm内径×375 μm外径,有效分离长度48 mm),并在254 nm处进行直接紫外检测。通过一系列优化,样品溶剂由NaOH(100 mmol/L)和ACN(1:1 v/v)组成,运行缓冲液由15 mmol/L硼酸钠-12.5 mmol/L磷酸二氢钠-42% v/v ACN(pH 10.1)组成,用于分离这四种蒽醌。分离快速且重现性高,所有四种化合物在6分钟内完全分离。样品通量率可达每小时12个。以峰高评估时,大黄素甲醚、大黄酚、芦荟大黄素和大黄素的重复性(定义为相对标准偏差)分别为4.45%、4.44%、4.34%、0.61%;以峰面积评估时,重复性分别为1.62%、0.89%、2.49%、2.19%。