续骨油的质量标准研究

Research on Quality Standard of Xugu Oil

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 scientific evidence for establishing research method on quality standard of Xugu oil.Methods：Rhubarb,lignum acronychiae,flos Rhododendri Mollis in Xugu oil were identified by thin layer chromatography（TLC）.Limit test for total alkaloid content in diester diterpenoid alkaloids（DDAs）（aconitine,hypaconitine,Mesaconitine）and content of Strychnine by high performance liquid chromatography（HPLC）.Detection mobile phase A of DDAs was acetonitriletetrahydrofuran（5：3）,mobile phase B was 0.1 mol/L ammonium acetic solution（add glacial acetic acid 0.5 mL per 1 000 mL）,detection wavelength was 238 nm.Detection mobile phase A of Strychnine was acetonitrile,mobile phase B was equivalent mixed solution of 0.01 mol/L sodium heptanesulfonate and 0.02 mol/L potassium dihydrogen phosphate（adjust the pH value to2.8 With 10%phosphoric acid）,detection wavelength was 260 nm.Results：Differentiation method of rhubarb,lignum acronychiae and flos Rhododendri Mollis were specific,average total alkaloid content of DDAs were 0.011 0 μg/mL,average content of strychnine was 0.620 6 μg/mL,did not exceed the specified requirements.Conclusion：Method for examination in the research is a simple,specific method with good reproducibility.It can provide scientific evidence for establishing quality standard of Xugu Oil.