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目的 建立高效液相色谱法测定戊己丸中吴茱萸碱和吴茱萸次碱含量的方法。方法 采用高效液相色谱法。IntersilC18分析色谱柱 (4.6mmID× 2 5 0mm ,粒径 5 μm) ,流动相 :乙腈 - 10 %乙腈 (5 0 :5 0 ) ,流速 :1ml/min ,检测波长 :2 2 5nm。 结果 吴茱萸碱和吴茱萸次碱的理论板数分别为 2 6 81和 2 0 6 7。吴茱萸碱回归方程 :Y =0 .0 76 4 6 +0 .0 0 0 0 0 0 196 5X ,r=0 .9999) ,线性范围 10 .2~ 5 1.0 μg·ml-1;吴茱萸次碱回归方程 :Y =- 0 .2 199+0 .0 0 0 0 0 0 36 5 8X ,r =0 .9999) ,线性范围 10 .0~ 5 0 .0 μg·ml-1。吴茱萸碱平均回收率为 97.3% ,RSD 3.2 % ,吴茱萸次碱平均回收率为 10 1.4 % ,RSD 3.9%。吴茱萸碱和吴茱萸次碱最低检出浓度分别为 0 .0 5和 0 .1μg·ml-1。结论 方法简便 ,结果准确。
Objective To establish a method for determination of evodiamine and rutaecarpine in Wuji Pill by high performance liquid chromatography. Method using high performance liquid chromatography. Intersil C18 analysis column (4.6mm ID × 250mm, particle size 5 μm), mobile phase: acetonitrile - 10% acetonitrile (50: 50), flow rate: 1 ml/min, detection wavelength: 225 nm. Results The theoretical plates of evodiamine and ruthenium were 286 and 207, respectively. The evodiamine regression equation: Y =0. 0 76 4 6 +0. 0 0 0 0 0 196 5X ,r=0.9999), with a linear range of 10. 2 to 5 1.0 μg·ml -1; The equation is: Y =- 0 .2 199+0 .0 0 0 0 0 36 5 8X ,r =0.9999). The linear range is from 1.0 to 5.00.0 μg·ml-1. The average recovery rate of evodiamine was 97.3%, RSD 3.2%, the average recovery rate of rutacarpine was 101.4%, and RSD was 3.9%. The lowest detection concentrations of evodiamine and rutacarpine were 0.5 and 0.1 μg·ml-1, respectively. Conclusion The method is simple and accurate.