不同生产工艺的戊己丸中吴茱萸碱和吴茱萸次碱含质量比较

Quality Comparison of Evodianmine and Rutaecarpine in Wuji Pills Using Different Production Process

目的:建立戊己丸中吴茱萸碱和吴茱萸次碱含质量的高效液相(HPLC)测定方法,并对超微戊己丸和常规戊己丸中吴茱萸碱和吴茱萸次碱的含质量进行比较。方法:采用色谱柱HypersilC18柱(4.6mm×250mm,5μm),流动相:乙腈水(48∶52),流速:1mL/min,检测波长:225nm。结果:吴茱萸碱和吴茱萸次碱的理论塔板数均大于3000,吴茱萸碱回归方程:A吴茱萸碱=107.73ρ-14.331,r=0.9999,线性范围1.02～20.4μg/mL;吴茱萸次碱回归方程:A吴茱萸次碱=15.596ρ-45.09,r=0.9998,线性范围4.4～176μg/mL。超微戊己丸中吴茱萸碱平均回收率为:99.61%,RSD为0.50%,质量分数为(0.096±0.0148)%;吴茱萸次碱平均回收率为94.85%,RSD为1.00%,质量分数为(0.343±0.0467)%。常规戊己丸中吴茱萸碱平均回收率为98.56%,RSD为1.70%,质量分数为(0.81±0.003)%;吴茱萸次碱平均回收率为99.55%,RSD为0.50%,质量分数为(0.161±0.0075)%。结论:超微戊己丸中吴茱萸碱和吴茱萸次碱的质量分数高于常规戊己丸。

Objective：To establish a HPLC method for the content of evodianmine and rutaecarpine in Wuji pills by HPLC,and to compare them between ultramicro Wuji pills and general Wuji pills.Methods：Chromatographic column：Hypersil C18（4.6 mm×250 mm,5 μm）,mobile phase：acetonitrile-water（48：52）,flow rate：1 mL/min,wavelength 225 nm.Results：The number of theoretical plates calculated by evodiamine and rutaecarpine peak was not below 3000.The regression equation of ultramicro evodiamine was A = 107.73 ρ-14.331,r = 0.999 9 and the linear range was 1.02-20.40 μg/mL.The regression equation of Ultramicro rutaecarpine was A = 15.596 ρ-45.09,r = 0.999 8 and the linear range was 4.4-176 μg/mL.The average recovery of ultramicro evodiamine was 99.61%（n = 5）,RSD 0.50%,and the mass fraction of ultramicro evodiamine was（0.096±0.0148）%.The average recovery of Ultramicro rutaecarpine was 94.85%（n = 5）,RSD 1.0%,and the mass fraction of ultramicro rutaecarpine was（0.343±0.0467）%.The average recovery of general evodiamine was 98.56%（n = 5）,RSD 1.70%,and the mass fraction of general evodiamine was（0.81±0.003）%.The average recovery of General rutaecarpine was 99.55%（n = 5）,RSD 0.50%,and the mass fraction of general rutaecarpine was（0.161±0.007 5）%.Conclusion：The mass fraction of evodiamine and rutaecarpine in ultramicro Wuji pills is higher than that of general Wuji pills.