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建立了以6种离子液体为萃取剂,超声辅助萃取结合高效液相色谱法同时测定昆明山海棠中雷公藤晋碱、雷公藤碱庚、雷酚内酯、雷公藤次碱和雷公藤醌A含量的方法。采用Inertsil ODS-4柱(4.6 mm×250 mm,3μm);以乙腈-0.1%磷酸溶液,梯度洗脱;检测波长220 nm;柱温30℃;流速0.75 m L·min-1。结果显示,提取雷酚内酯、雷公藤醌A时最佳萃取条件为0.6 mol·L-1[BMIm]PF6甲醇溶液,固液比为1∶10,分别在0.000 65~0.026,0.066 55~2.662μg呈良好的线性关系(r=0.999 9),平均回收率分别为102.4%,97.90%,RSD分别为2.5%,1.5%;提取雷公藤晋碱、雷公藤碱庚和雷公藤次碱的最佳萃取条件为0.6 mol·L-1[BMIm]PF6无水乙醇溶液,固液比为1∶10,分别在0.023 9~0.956,0.002 7~0.108,0.006 4~0.256μg呈良好的线性关系(r=0.999 9),平均回收率分别为100.6%,99.50%,98.70%,RSD分别为2.1%,1.9%,2.7%。实验表明该方法操作简单,准确可靠,重复性好,且绿色环保,为昆明山海棠的质量控制提供了一种可靠的分析方法。
A method for the simultaneous determination of Tripterygium wilfordii, Tripterygium Hypoglaucum, Tripterololide, Tripterygium wilfordii and Tripterine quinone A in Kunming Begonia was established by using six kinds of ionic liquids as extractant and ultrasonic assisted extraction combined with high performance liquid chromatography Method of content. The column was eluted with an Inertsil ODS-4 column (4.6 mm × 250 mm, 3 μm). The sample was eluted with a gradient of acetonitrile-0.1% phosphoric acid solution. The detection wavelength was set at 220 nm. The column temperature was 30 ℃ and the flow rate was 0.75 m L · min-1. The results showed that the optimum extraction conditions for the extraction of triptolide and triptolide were 0.6 mol·L-1 [BMIm] PF6 methanol solution, the solid-liquid ratio was 1:10, respectively, at 0.000 65 ~ 0.026,0.066 55 ~ (R = 0.999 9). The average recoveries were 102.4% and 97.90%, respectively. The RSDs were 2.5% and 1.5%, respectively. The extraction rates of tripterygium wilfordii, tripterygium wilfordii and tripterygium wilfordii The optimum extraction conditions were 0.6 mol·L-1 [BMIm] PF6 absolute ethanol solution, the solid-liquid ratio was 1:10, showing a good linear relationship between 0.023 9 ~ 0.956, 0.002 7 ~ 0.108, 0.006 4 ~ 0.256μg (r = 0.999 9). The average recoveries were 100.6%, 99.50% and 98.70%, respectively. The RSDs were 2.1%, 1.9% and 2.7% respectively. Experiments show that the method is simple, accurate and reliable, good repeatability, and green, providing a reliable analytical method for the quality control of Begonia.