摘要
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。
Using six kinds of ionic liquids as extractants,ultrasonic-assisted extraction coupled with HPLC method was developed for the simultaneous determination of wilforgine,wiforizine,triptophenolide,wilforine and triptoquinone A in Tripterygium hypoglaucum. The separation was performed on an Inertsil ODS-4 column with the mobile phase of acetonitrile-0. 1% phosphoric acid in gradient elution at a flow rate of 0. 75 m L·min-1. Detection wavelength was 220 nm and the column temperature was 30℃. Under the optimal extractions,the results showed that triptophenolide and triptoquinone A had the highest extraction yield by using 0. 6 mol · L-1[BMIm]PF6methanol solution as extraction solvent with the solid-liquid ratio of 1 ∶ 10. The calibration curves of triptophenolide and triptoquinone A showed a good linearity in the range of 0. 000 65-0. 026,0. 066 55-2. 662 μg（ r = 0. 999 9） respectively. The average recovery was 102. 4% and 97. 90% with RSD of 2. 5% and 1. 5%,respectively. Wilforgine,wiforizine and wilforine had the highest extraction yield when using 0. 6 mol· L-1[BMIm]PF6absolute ethanol solution as extraction solvent with the solid-liquid ratio of 1∶10. The content of wilforgine,wiforizine and wilforine from 0. 023 9-0. 956,0. 002 7-0. 108,0. 006 4-0. 256 μg showed a good linearity（ r = 0. 999 9）,and the average recovery was 100. 6%,99. 50% and 98. 70% with RSD of 2. 1%,1. 9% and 2. 7%,respectively.The results indicated that this method is convenient,reliable and green,and can be used as a reliableanalytical method for the quality control of T. hypoglaucum.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2016年第5期879-886,共8页
China Journal of Chinese Materia Medica
基金
重庆市科委应用开发(重大)项目(cstc2013jcsf10011
cstc2014yykf C10005)
重庆市青年科技人才培养计划项目(cstc2014kjrc-qnrc10006)
