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目的:了解乌头类中药中新乌头碱、乌头碱、次乌头碱、新乌头次碱四种有效成分的含量,为临床提供研究依据。方法:采用高效液相色谱法进行各种有效成分的测定,色谱柱为Agilent Zobax XDB C18(250.0×2.1mm,5um),流动相为0.01%氨水溶液-乙腈,流速1ml/min,检测波长240nm,采用LC-MS~n法进行生物碱成分的初步鉴定,了解各种成分的含量,将4种生物碱进行加热,分析受热稳定曲线变化情况,给家兔灌服附子,测定入血成分。结果:新乌头次碱的热稳定性更好,更适合作为药效指标成分,以新乌头次碱作为乌头类中药有效成分的测定指标,进样量在0.51~10.2ug范围内与峰面积积分值呈良好线性关系(r=0.9998);平均回收率为102.1%,RSD=2.2%(n=6)。结论:新乌头次碱作为乌头类中药中的有效成分,具有热稳定性好,可作为入血成分,具有良好的检测价值,可作为乌头类中药含量检测、赝品区分的有效指标。
Objective: To understand the contents of four active constituents of aconitine, aconitine, hypaconitine and mesaconitine in aconite traditional Chinese medicine, and to provide the basis for clinical research. Methods: The determination of various active ingredients was carried out by high performance liquid chromatography with Agilent Zobax XDB C18 column (250.0 × 2.1 mm, 5 μm), mobile phase of 0.01% aqueous ammonia solution, acetonitrile flow rate of 1 ml / min, detection wavelength of 240 nm , The initial identification of alkaloid components was carried out by LC-MS ~ n method, and the contents of various components were determined. The four alkaloids were heated, the changes of heat-stable curves were analyzed, and the aconites were drenched into the rabbits to determine the inflow components. Results: The new aconitine alkali thermal stability is better, more suitable as an index of efficacy parameters, the new aconitine alkaloids as the active ingredient in the determination of aconitine index injection volume in the range of 0.51 ~ 10.2ug with The peak area integral value showed a good linear relationship (r = 0.9998); the average recovery was 102.1%, RSD = 2.2% (n = 6). Conclusion: As a new aconitine alkaloids active ingredients in Chinese medicine, has good thermal stability, can be used as a blood component, has a good detection value, can be used as Aconitum Chinese medicine content detection, counterfeiting an effective indicator of distinction.