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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 investigate the HPLC method for determination of rhynchophylline and isorhamnetine in Uncaria. Methods: HPLC method was used to determine the content of rhynchophylline and isoniazid in Uncaria rhynchophylla. HPLC-ESI-MS was used to study the chemical composition of rhynchophylline and isorhamine Component conversion. Results: The linear relationship of rhynchophylline with 0.064-5.100 mg was good and the precision was good. When the samples were extracted by reflux, the average recoveries were 87.51% ~ 88.83% and the recovery rates were 12.60%. When the samples were extracted by ultrasonic, The recoveries of samples ranged from 99.48% to 103.2%. The extraction recovery rate was 47.08%. When the samples were extracted by reflux, the average recoveries were 107.9% ~ 113.9% and the recovery rates were 40.00%. When the samples were extracted by ultrasonic, the average was The recovery rate was 97.00% ~ 99.59%, extraction recovery rate was 51.03%. Mass spectrometry results showed that the reason for the unacceptable recovery rate was that most of rhynchophylline was converted to isorhamine during the extraction process and a small part was converted into unknown components; isoniazid was converted to rhynchophylline Rhynchophylline, isoborneol and 22-O-β-D-glucopyranosyl isocorynoxeinic acid four kinds of ingredients. Conclusion: The determination of rhynchophylline and isorhamnetin in Uncaria rhynchophylla by HPLC should be performed by ultrasonic extraction, and the recovery rate should be paid attention to.