炮天雄质量标准研究

Study on the Quality Standard for Processed Aconitum Carmichnaeli

目的： 建立炮天雄的质量标准。 方法： 采用薄层色谱法对苯甲酰新乌头原碱进行定性研究;采用高效液相色谱方法，选用Eclipse XDB-C18色谱柱（4.6 mm250 mm，5 μm），柱温35℃，流动相A为0.1 molL-1醋酸铵溶液（每1 000 mL加冰醋酸0.5 mL），B为四氢呋喃-乙腈（15∶25），梯度洗脱，体积流量1 mLmin-1，检测波长235 nm。 结果： 炮天雄中水分为10.1%~12.3%;定性鉴别专属性强;苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、次乌头碱和乌头碱分别在0.049 4~1.976，0.023 32~0.932 8，0.049 95~1.998，0.024 46~0.978 56，0.024 91~0.996 48，0.022 02~0.880 8 μg进样量呈良好线性关系，r均为0.999 9;平均回收率分别为98.79%，100.66%，97.06%，97.91%，103.58%，102.77%;RSD分别为1.90%，2.23%，1.91%，1.96%，1.08%，2.19%。 结论： 该方法操作简便，结果准确，可作为炮天雄的质量控制方法。

Objective： To establish the quality standards for Chinese medicine processed Aconitum carmichneli （Tuber of Aconitum armichaeli）. Method： Benzoylmesaconine was identified by TLC method. Monoester alkaloids and diester type alkaloids were determined by HPLC method. HPLC condition was as follows：The Eclipse XDB-C18 （4.6 mm250 mm,5 μm） column was used;the column temperature was maintained at 35℃. The mobile phase system was 0.1 mol L-1 ammonium acetate （per 1 000 mL contains 0.5 mL glacial acetic acid,phase A） and tetrahydrofuran-acetonitrile （15：25,phase B） with gradient elution. The flow rate was 1 mL min-1. The detection wavelength was set at 235 nm. Result： The water content was ranged from 10.1% to 12.3%. The qualitative identification was specific. Benzoylmesaconine,benzoylaconine,benzoylhypaconine,mesaconitine,hypaconitine and aconitine showed good linear relationship in the range of 0.049 4-1.976,0.023 32-0.932 8,0.049 95-1.998,0.024 46-0.978 56,0.024 91-0.996 48,0.022 02-0.880 8 μg respectively （r=0.999 9 for all six substances）. The average recovery rates of benzoylmesaconine,benzoylaconine,benzoylhypaconine,mesaconitine and hypaconitine were 98.79%,100.66%,97.06%,97.91%,103.58% and 102.77% respectively with RSD of 1.90%,2.23%,1.91%,1.96%,1.08% and 2.19% respectively. Conclusion： The method is simple,reproducible and accurate;it can be used as the quality control methods of the Chinese medicine processed Aconitum carmichaeli.