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目的:为建立续骨油的质量标准研究方法提供科学依据。方法:采用薄层色谱法对续骨油中大黄、降香和闹羊花作定性鉴别,采用高效液相色谱法对双酯型生物碱(乌头碱、次乌头碱、新乌头碱)总碱含量及士的宁含量作限量检查,双酯型生物碱的检测流动相A是乙腈-四氢呋喃(5∶3),流动相B是0.1 mol/L醋酸铵溶液(每1 000 mL加冰醋酸0.5 mL),检测波长为235 nm;士的宁的检测流动相A是乙腈,B是0.01 mol/L庚烷磺酸钠与0.02 mol/L磷酸二氢钾等量混合溶液(用10%磷酸调节PH值2.8);检测波长为260 nm。结果:大黄、降香、闹羊花的鉴别方法专属性强,双酯型生物碱(乌头碱、次乌头碱、新乌头碱)总碱平均含量为0.011 0μg/mL,士的宁的平均含量为0.620 6μg/mL,均未超过规定要求。结论:所建立的检验方法操作简便,专属性强,重现性较好,可为续骨油质量标准的建立提供科学依据。
Objective: To provide a scientific basis for the establishment of the research method of quality standards for continued bone oil. Methods: The quality of Rhizoma Dioscoreae, Rhizoma Dioscoreae and Rhododendron macula were evaluated by thin-layer chromatography (TLC), and the contents of double ester alkaloids (aconitine, hypaconitine, mesaconitine ), Total alkaloids content and strychnine content as the limit check, detection of diester alkaloids mobile phase A is acetonitrile-tetrahydrofuran (5: 3), mobile phase B is 0.1 mol / L ammonium acetate solution Acetic acid 0.5 mL) at a detection wavelength of 235 nm. The mobile phase A of strychnine was acetonitrile, B was a mixed solution of 0.01 mol / L sodium heptane sulfonate and 0.02 mol / L potassium dihydrogen phosphate % Phosphoric acid to adjust PH value 2.8); detection wavelength is 260 nm. Results: The identification methods of Rhubarb, Rhodiola, Amuropathie excelsior, the average content of total alkaloids of double ester alkaloids (aconitine, hypaconitine and mesaconitine) is 0.011 0μg / mL, strychnine The average content of 0.620 6μg / mL, did not exceed the required requirements. Conclusion: The established test method is simple, specific and reproducible, which can provide a scientific basis for the establishment of continuous bone oil quality standards.