Yu Lijun, Xu Yan, Feng Huatao, Li Sam Fong Yau
Department of Chemistry, National University of Singapore, Singapore, Republic of Singapore.
Electrophoresis. 2005 Sep;26(17):3397-404. doi: 10.1002/elps.200500233.
A simple and rapid micellar electrokinetic chromatography (MEKC) method was developed for the separation and determination of four toxic pyrrolizidine alkaloids (PAs) (senkirkine, senecionine, retrorsine, and seneciphylline) in two traditional Chinese herbal medicines (Qian liguang and Kuan donghua). Separation was performed in the running buffer consisting of 20 mM borate, 30 mM SDS, and 20% methanol at pH 9.1. With the optimized separation conditions, four PAs were separated in 17 min by a single run. The calibration curves showed good linearity with correlation efficiencies (R(2)) between 0.9940 and 0.9988. RSDs in migration time and peak area were 0.31, 0.40, 0.39, 0.48% and 3.28, 3.48, 4.16, 3.42% for senkirkine, senecionine, retrorsine, and seneciphylline, respectively. Limits of detection (S/N = 3) varied from 1.19 to 2.70 microg/mL. The proposed method was applied to determine the PAs extracted from Chinese herbal medicines (Qian liguang and Kuan donghua). PA of senkirkine in Kuan donghua was detected and the amount was found to be 79.1 microg/g. The results obtained indicate that the proposed MEKC method could potentially become an effective alternative tool for qualification control and quantitative analysis of herbal medicines in pharmaceutical industry.
建立了一种简单快速的胶束电动毛细管色谱法（MEKC），用于分离和测定两种中药材（千里光和款冬花）中的四种有毒吡咯里西啶生物碱（PAs）（Senkirkine、Senecionine、Retrorsine和Seneciphylline）。在由20 mM硼酸盐、30 mM十二烷基硫酸钠（SDS）和20%甲醇组成的pH 9.1的运行缓冲液中进行分离。在优化的分离条件下，一次进样在17分钟内分离出四种PAs。校准曲线显示出良好的线性，相关系数（R²）在0.9940至0.9988之间。Senkirkine、Senecionine、Retrorsine和Seneciphylline迁移时间和峰面积的相对标准偏差分别为0.31%、0.40%、0.39%、0.48%和3.28%、3.48%、4.16%、3.42%。检测限（S/N = 3）在1.19至2.70 μg/mL之间。所提出的方法用于测定从中药材（千里光和款冬花）中提取的PAs。检测到款冬花中Senkirkine的PA，含量为79.1 μg/g。所得结果表明，所提出的MEKC方法有可能成为制药行业中药材质量控制和定量分析的有效替代工具。
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