基于超声辅助离子液体结合高效液相色谱法同时测定粉背雷公藤中5种化合物

[Simultaneous determination of 5 compounds in Tripterygium hypoglaucum based on ultrasound-assisted ionic liquid coupled with HPLC].

作者信息

Zhang Xiao-Mei, Chen Yi-Long, Yao Yuan-Yuan, Li Na, Liu You-Ping, Liang Xu-Ming

机构信息

Chengdu University of Traditional Chinese Medicine, Chengdu 611137, China.

Chongqing Academy of Chinese Traditional Materia Medica, Chongqing 400065, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2016 Mar;41(5):879-886. doi: 10.4268/cjcmm20160520.

DOI:10.4268/cjcmm20160520

PMID:28875643

Abstract

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 mL•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]PF6 methanol 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.

摘要

以6种离子液体为萃取剂，建立了超声辅助萃取结合高效液相色谱法同时测定粉背雷公藤中雷公藤吉碱、雷公藤晋碱、雷公藤酚甲、雷公藤碱和雷公藤醌A的方法。采用Inertsil ODS-4色谱柱，以乙腈-0.1%磷酸为流动相进行梯度洗脱，流速为0.75 mL•min⁻¹。检测波长为220 nm，柱温为30℃。在最佳萃取条件下，结果表明，以0.6 mol•L⁻¹ [BMIm]PF6甲醇溶液为萃取溶剂，固液比为1∶10时，雷公藤酚甲和雷公藤醌A的萃取率最高。雷公藤酚甲和雷公藤醌A的校准曲线在0.000 65 - 0.026、0.066 55 - 2.662 μg范围内线性关系良好（r = 0.999 9）。平均回收率分别为102.4%和97.90%，相对标准偏差分别为2.5%和1.5%。以0.6 mol•L⁻¹ [BMIm]PF6无水乙醇溶液为萃取溶剂，固液比为1∶10时，雷公藤吉碱、雷公藤晋碱和雷公藤碱的萃取率最高。雷公藤吉碱、雷公藤晋碱和雷公藤碱的含量在0.023 9 - 0.956、0.002 7 - 0.108、0.006 4 - 0.256 μg范围内线性关系良好（r = 0.999 9），平均回收率分别为100.6%、99.50%和98.70%，相对标准偏差分别为2.1%、1.9%和2.7%。结果表明，该方法简便、可靠、绿色，可作为粉背雷公藤质量控制的可靠分析方法。