摘要
目的:建立青风藤中青藤碱和木兰花碱的含量测定方法,并用于评价市售青风藤的质量。方法:采用高效液相色谱法,色谱柱为Synergi Polar-RP苯基C18柱(250 mm×4. 6 mm,4"m),流动相为乙腈(B)-1%乙酸水溶液(A),梯度洗脱(0~15 min,10%→15%B; 15~17 min,15%→20%B; 17~22 min,20%→40%B; 22~30 min,40%→40%B),柱温为30℃;检测波长为280 nm,流速为1 m L·min-1。结果:本方法的精密度、准确度和重现性的RSD皆小于2%,青藤碱和木兰花碱在0. 01~0. 40 mg·m L-1线性关系良好;在测定的62批样品中,除了4批伪品之外,只有1批样品中青藤碱含量低于《中华人民共和国药典》要求,青藤碱和木兰花碱的含量分别为0. 236%~4. 735%和0. 256%~3. 682%。结论:本方法精密度、准确度和重现性良好,适用于青风藤中青藤碱和木兰花碱的含量测定;大多数市售青风藤的质量符合《中华人民共和国药典》要求,但主要成分青藤碱和木兰花碱的含量存在差异。
Objective : To establish a HPLC assay method for sinomenine and magnoflorine in Caulis Sinomenii, and employ it to evaluate the quality of Caulis Sinomenii eomnlercially available in China. Methods : The analysis was performed on a Synergi Polar-RP Phenomenex C18 column(250 mm x 4. 6 mm, 4 μm using aeetonitrile(A) -1% acetic acid solution(B) as the mobile phase with gradient elution(0-15 min, 10%-15% B; 15-17 min, 15%-20% B; 17-22 min, 20%-40% B; 22-30 min, 40%-40% B). The column temperature was set at 30 ℃, the UV detection wavelength was 280 nm and the flow rate was 1.0 mL .min -1. Results: The RSDs for precision, accuracy, and repeatability tests were all less than 2%. Sinome- nine and magnoflorine showed good linearity in the concentration range of 0. 014). 40 mg · mL. In the 62 batches of samples tested, except 4 batches which were determined as adulterants, only 1 batch the sinomenine content was less than the lower limit required by Chinese Pharmacopeia. The content of sinomenine ranged from 0. 236% to 4. 735%, and that of magnoflorine ranged from 0. 256% to 3. 682%. Conclusion: This method has good precision, accuracy and repeatability, and it is suitable for determination of the two substances in Caulis Sinomenii. The quality of most Caulis Sinomenii commercially available in Chinese market cotfforms to the requirements of Chinese Pharmacopoeia despite existed qualitative differences.
作者
王青青
方明月
刘双月
李德利
马超
孙爱东
王如峰
WANG Qing-qing;FANG Ming-yue;LIU Shuang-yue;LI De-li;MA Chao;SUN Ai-dong;WANG Ru-feng(School of Life Sciences,Beijing University of Chinese Medicine,Beijing 102488,China;College of Biological Scie~wes and Technology,Beijing Forestry University,Beijing 100083,China)
出处
《中国现代中药》
CAS
2018年第11期1367-1371,共5页
Modern Chinese Medicine
基金
林业公益性行业科研专项经费项目(201504606)