摘要
目的:探讨钩藤中钩藤碱和异钩藤碱的HPLC含量测定方法。方法:采用RP-HPLC,对钩藤中钩藤碱和异钩藤碱的HPLC含量测定方法学进行考察,同时采用HPLC-ESI-MS研究钩藤碱和异钩藤碱在加热过程中的化学成分转化情况。结果:钩藤碱在0.064～5.100 mg线性关系良好,精密度良好;当样品采用回流提取时,平均加样回收率87.51%～88.83%,提取回收率12.60%;当样品采用超声提取时,平均加样回收率99.48%～103.2%,提取回收率47.08%。异钩藤碱在0.064～5.110 mg线性关系良好,精密度良好;当样品采用回流提取时,平均加样回收率107.9%～113.9%,提取回收率40.00%,当样品采用超声提取时,平均加样回收率97.00%～99.59%,提取回收率51.03%。质谱分析结果表明回收率不合格的原因是钩藤碱在提取过程中大部分转化为异钩藤碱,有一小部分转化为未知成分;异钩藤碱在提取过程中转化为钩藤碱、去氢钩藤碱、异去氢钩藤碱及22-O-β-D-glucopyranosyl isocorynoxeinic acid 4种成分。结论:HPLC测定钩藤中钩藤碱和异钩藤碱宜采用超声提取法,并应注意回收率问题。
Objective： To explore an HPLC method for determination of rhnchophylline and isorhnchophylline in Uncaria rhn- chophylla. Method： An HPLC method has been developed for determination of rhnehophylline and isorhnchophylline. The transforma- tion of rhnchophylline and isorhnchophylline after heating was also studied by HPLC-ESI-MS. Result： Good linearities of rhynchophyl- line and isorhynchophylline were 0. 064-5. 100, 0. 064-5. 110 mg, respectively. The average recoveries were from 87.51% to 88.83% for rhynehophylline and from 107.9% to 113.9% for isorhynchophylline. The recoveries of rhynchophylline and isorhnchophylline ref- erence solutions after extraction were 12. 60% and 40.00% in the reflux extraction procedure, respectively. While in the ultrasonic ex- traction procedure, the average recoveries of rhynehophylline and isorhynchophylline was from 99.48% to 103.2% and from 97.00% to 99.59% , resepeetively. The recoveries of rhynehophylline and isorhnchophylline reference solutions after extraction were 47. 08% and 51.03%, respectively. The unqualified recovery could be elucidated by HPLC-ESI-MS analysis, indicating that trhynchophylline could be transformed mostly into isorhynchophylline and a little amount of unkown composition, while isorhynchophylline could be transformed into rhynchophylline isocorynoxeine, corynoxeine and 22-O-β-D-glucopyranosyl isocorynoxeinic acid during the extraction procedure. Conclusion： Ultrasonic extraction procedure was more sutble for HPLC determination of the content of rhynchophylline and isorhynehophylline in U. rhnchophylla, however, the recovery problems should be paid attention to when it comes to the determination.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2013年第5期720-724,共5页
China Journal of Chinese Materia Medica
基金
上海市科委中药现代化专项(10DZ1973000)
上海市自然科学基金项目(09ZR1429600)
上海市教委创新项目(10YZ57)
上海市教委重点学科项目(J50302)
关键词
钩藤
钩藤碱
异钩藤碱
HPLC
Uncaria rhynchophylla
rhynchophylline
isorhynchophylline
HPLC
