HPLC测“半蒌贝蔹芨攻乌”中乌头与其它诸药合煎前后次乌头碱的含量变化

 目的　建立“半蒌贝蔹芨攻乌”中乌头剧毒成分(次乌头碱 )的HPLC定量测定方法。对其中的乌头与其它诸药配伍前后水煎剂中次乌头碱的含量进行测定,探讨“半蒌贝蔹芨攻乌”的科学性。方法　HPLC条件:流动相:甲醇-水-氯仿-三乙胺(70∶30∶2∶0.2),流速1.0mL·min^-1,检测波长235nm,柱温40℃;选取生附片(属乌头类)单煎及分别与半夏、全瓜蒌、浙贝母、白蔹、白芨1∶1配伍合煎,100℃水浴加热45min制备水煎剂,乙醚萃取煎液中的待测成分,氮气流吹干萃取剂,残渣用甲醇溶解后进样测定次乌头碱含量。结果　除半夏外,其它诸药与乌头配伍均能使水煎剂中次乌头碱的含量增高,且与药材中的酸性成分(溶液pH值下降)有关。结论　本实验从诸药与生附片合煎液中有毒化学成分含量升高角度,肯定了“半蒌贝蔹芨攻乌”的科学性。

Determination of content changes of hypaconitine in preparations of aconite matching other herbs in "pinellia tuber,snakegourd fruit,fritillaria,japanese ampelopsis root and common bletilla tuber counteract aconite" by HPLC

OBJECTIVE To develop a HPLC method for the determination of hypaconitine,toxic component from aconite,and to detect the content changes of hypaconitine in preparations of aconite compounded with pinellia tuber,whole snakegourd fruit,fritillaria,japanese ampelopsis root and common bletilla tuber so as to probe the counteractive mechanism of aconite and others herbs,which are herbal counteractors.METHODS The mixture of CH₃OH-H₂O-CHCl₃(C₂H₅)₃N(70∶30∶2∶0.2) was used as the mobile phase,the flow rate was 1.0mL·min^-1 with the detection wavelength at 235 nm and the column temperature at 40℃.Aconitum carmichaelii Debx.(one of aconite) was selected to be singly treated or mixed with Pinellia ternata(Thunb.) Breit.,Trichosanthes kiritowii Maxim.,Fritillaria thunbergii MiQ.,Ampelopsis japonica(Thunb.) Makino.And Bletilla striata(Thunb.) Reichb.f.respectively at ratio of 1∶1,then heated by boiling water 45 min to make decoction.RESULT The content of hypaconitine in decoction of aconite compounded with whole snakegourd fruit,fritillaria,japanese ampelopsis root and common bletilla tuber was far higher than that in decoction of single aconite,and the result was related to acidic components (the pH value descend in decoctions) in whole snakegourd fruit,fritillaria,etc.CONCLUSION The experiment affirmed the theory of “pinellia tuber,snakegourd fruit,fritillaria,japanese ampelopsis root and common bletilla tuber counteract aconite” in point of chemical view.