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目的:采用高效液相色谱法检测在胆巴溶液中浸泡不同时间的附子中6种生物碱的含量,分析附子中生物碱成分随浸泡时间的变化规律。方法:采用Waters sunfire C18色谱柱(4.6 mm×250 mm,5μm),流速0.8 mL·min-1,柱温30℃,检测波长235 nm,流动相乙腈-四氢呋喃(25∶15)和0.1 mol·L-1醋酸铵溶液(每1 000 mL加冰醋酸0.5 mL),梯度洗脱。结果:泥附子洗净后在胆巴溶液中浸泡,新乌头碱、次乌头碱、乌头碱和苯甲酰新乌头原碱的含量逐渐降低,浸泡20 d后,成分变化趋于平缓。浸泡20 d样品与生品比较,其降低率分别为60.39%,73.84%,72.57%和88.46%。结论:泥附子洗净后在胆巴溶液中浸泡,能达到防止腐烂的目的,浸泡20 d以后胆附子质量稳定,同时双酯型和单酯型生物碱总量均流失70%左右,为保证临床用药的安全和有效,有必要改进泥附子产地加工方法。
OBJECTIVE: To determine the content of six alkaloids in aconite root of soaking in different times in gall solution by high performance liquid chromatography (HPLC), and to analyze the change rule of alkaloid content in aconite with soaking time. METHODS: Waters sunfire C18 column (4.6 mm × 250 mm, 5 μm) was used at a flow rate of 0.8 mL · min-1 at a detection wavelength of 235 nm with acetonitrile-tetrahydrofuran (25:15) L-1 ammonium acetate solution (0.5 mL per 1 000 mL glacial acetic acid), gradient elution. Results: The content of mesaconitine, hypaconitine, aconitine and benzoyl mesaconitine decreased gradually after immersion in the solution of gall, gentle. Compared with the raw samples, the decreasing rates of soaking 20 d samples were 60.39%, 73.84%, 72.57% and 88.46% respectively. CONCLUSION: After the aconite was washed, it was immersed in the solution of the gall to achieve the purpose of preventing decay. After 20 days of immersion, its quality was stable, while the total amount of the diester and monoester alkaloids lost about 70% Clinical medication is safe and effective, it is necessary to improve the processing method of mud appendage origin.