HPLC测定蒙药材草乌叶中4种双酯型二萜生物碱含量  

Content determination of four diester diterpenoid alkaloids in leaves of Aconitum kusnezoffii by HPLC

作　　者：昝珂[1] 旺杰次仁 鲁静[1] 过立农[1] 郑健[1] 马双成[1] ZAN Ke;WANGJIE Ci-ren;LU Jing;GUO Li-nong;ZHENG Jian;MA Shuang-eheng(National Institutes for Food and Drug Control, Beijing 100050, China;Tibet lnstitt~te for Food and Drt~g Control, Lhasa 850000, China)

机构地区：[1]中国食品药品检定研究院,北京100050 [2]西藏自治区食品药品检验研究院,西藏拉萨850000

出　　处：《中国中药杂志》2018年第4期766-771,共6页China Journal of Chinese Materia Medica

基　　金：国家“重大新药创制”科技重大专项(2014ZX09304307-002)

摘　　要：建立同时测定蒙药草乌叶中4种双酯型二萜生物碱北草乌碱、新乌头碱、次乌头碱和乌头碱含量的色谱方法，用于指导草乌叶的质量控制。以北草乌碱、新乌头碱、次乌头碱和乌头碱为对照品，采用Waters XBridgeC18色谱柱（4．6mm×250mm，5μm），乙腈（A）40mmol·L^-1醋酸铵水溶液（B，氨水调pH至10．5）（33：67）为流动相；流速1．0mL·min^-1；检测波长为235nm；柱温30℃；进样量10μL。12批草乌叶中北草乌碱、新乌头碱、次乌头碱和乌头碱质量分数分别为0．0255-0．0885，0．0391-0．0715，0．0266～0．0810，0．00812～0．0312mg·g^-1。同时考察了不同采收期草乌叶药材中这4种成分含量的影响，随着采收期的推迟，含量先减后增。该研究可用于草乌叶药材中双酯型二萜生物碱的含量测定，为该药材质量标准的完善提供参考，初步阐明了草乌叶毒性和采收期的科学内涵。This present study is to develop an HPLC method for simultaneous determination of four diester diterpcnoid alkaloids, beiwutine, mesaconitine, hypaconitine and aconitine in the leaves of Aconitun kusnezoffii, so as to provide evidence of the quality con- trol of this herb. The four constituents were measured on a Waters XBridge Clscolumn （4. 6 mm x250 mm, 5 μm）. The mobile phase was acetonitrile-40 mmol·L-1ammonium acetate solution （adjusted pH to 10. 5 with ammonia solution） （33：67） with isocratic elution at a flow rate of＇ 1.0 mL·min-1 ; the detection wavelength was 235 rim; the column temperature was 30 ℃, and the injection volume was 10 μL. Next, this contents of the four diester diterpenoid alkaloids in 12 samples were 0. 025 5-0. 088 5, 0. 039 1-0. 071 5, 0. 026 6-0. 081 0 and 0. 008 12-0. 031 2 mg.g^-1 , respectively. Next, this method has been successfully applied to the analysis of A. kusnezoffii foliura in different harvest periods. The contents of the four alkaloids decreased primarily, and then increased with the post- poning of harvest. The established method is proved to be accurate and sensitive for the determination of alkaloids in A. kusnezoffii foli- um, and may be useful for the quality improvement of this herbal medicine. Moreover, these results indicated the scientific significance for the toxicity and the suitable harvest time of this herb.

关 键 词：草乌叶 北草乌碱 新乌头碱 次乌头碱 乌头碱 含量测定 毒性 最佳采收期 

分 类 号：O657.72[理学—分析化学] R29[理学—化学]