Yang Xiu-Juan, Hong Yan-Long, Wu Fei, Ruan Ke-Feng, Feng Yi
Engineering Research Center of Modern Preparation Technology of Traditional Chinese Medicine, Ministry of Education, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China.
Zhongguo Zhong Yao Za Zhi. 2013 Mar;38(5):720-4.
To explore an HPLC method for determination of rhnchophylline and isorhnchophylline in Uncaria rhnchophylla.
An HPLC method has been developed for determination of rhnchophylline and isorhnchophylline. The transformation of rhnchophylline and isorhnchophylline after heating was also studied by HPLC-ESI-MS.
Good linearities of rhynchophylline and isorhynchophylline were 0.064-5.100, 0.064-5.110 mg, respectively. The average recoveries were from 87.51% to 88.83% for rhynchophylline and from 107.9% to 113.9% for isorhynchophylline. The recoveries of rhynchophylline and isorhnchophylline reference solutions after extraction were 12.60% and 40.00% in the reflux extraction procedure, respectively. While in the ultrasonic extraction procedure, the average recoveries of rhynchophylline and isorhynchophylline was from 99.48% to 103.2% and from 97.00% to 99.59%, resepectively. The recoveries of rhynchophylline 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-beta-D-glucopyranosyl isocorynoxeinic acid during the extraction procedure.
Ultrasonic extraction procedure was more sutble for HPLC determination of the content of rhynchophylline and isorhynchophylline in U. rhnchophylla, however, the recovery problems should be paid attention to when it comes to the determination.
探索一种用于测定钩藤中钩藤碱和异钩藤碱的高效液相色谱法。
建立了一种测定钩藤碱和异钩藤碱的高效液相色谱法。还通过高效液相色谱-电喷雾电离质谱法研究了加热后钩藤碱和异钩藤碱的转化情况。
钩藤碱和异钩藤碱的良好线性范围分别为0.064 - 5.100、0.064 - 5.110 mg。钩藤碱的平均回收率为87.51%至88.83%，异钩藤碱的平均回收率为107.9%至113.9%。在回流提取过程中，钩藤碱和异钩藤碱对照品溶液提取后的回收率分别为12.60%和40.00%。而在超声提取过程中，钩藤碱和异钩藤碱的平均回收率分别为99.48%至103.2%和97.00%至99.59%。钩藤碱和异钩藤碱对照品溶液提取后的回收率分别为47.08%和51.03%。提取后回收率不合格的情况可通过高效液相色谱-电喷雾电离质谱分析来阐明，表明钩藤碱在提取过程中大部分可转化为异钩藤碱和少量未知成分，而异钩藤碱可转化为钩藤碱、异去甲氧基钩藤碱、去甲氧基钩藤碱和22 - O - β - D - 吡喃葡萄糖基异去甲氧基钩藤碱酸。
超声提取法更适合用于高效液相色谱法测定钩藤中钩藤碱和异钩藤碱的含量，然而，在测定时应注意回收率问题。
