高效液相色谱法同时测定制吴茱萸及其提取物中吴茱萸碱、吴茱萸次碱和吴茱萸内酯含量

Simultaneous Determination of Evodiamine,Rutaecarpine and Evodin in Cut Crude Drug and Exact of Fructus Evodiae by High-performance Liquid Chromatography

目的:建立高效液相色谱法同时测定制吴茱萸及其提取物中吴茱萸碱、吴茱萸次碱和吴茱萸内酯含量的方法。方法:采用高效液相色谱法,Kromasail C18色谱柱(4.6 mm×250 mm,5μm);流动相:乙腈-水-四氢呋喃-乙酸(51∶48∶1∶0.1),流速:1 mL.min-1;检测波长:225 nm:柱温:32℃。结果:吴茱萸碱回归方程:Y吴茱萸碱=10 300 000X-14 700,r=0.999 9,线性范围0.015～0.3μg;吴茱萸次碱回归方程:Y吴茱萸次碱=5 380 000X-6 610,r=0.999 9,线性范围0.012～0.24μg;吴茱萸内酯回归方程:Y吴茱萸内酯=227 000X-5 110,r=0.999 6,线性范围0.059～1.18μg。吴茱萸碱平均回收率为99.6%,RSD 0.65%;吴茱萸次碱平均回收率为99.1%,RSD1.2%;吴茱萸内酯平均回收率为97.5%,RSD1.4%。结论:方法简便,结果准确。

Objective： To develop an HPLC method to determine evodiamine, rutaecarpine and evodin simultaneously in cut crude drug and exact of fructus evodiae. Methods：The separation was performed on the Kromasail C18 （4.6 mm × 250 mm, 5 μm） column with acetonitrile-water-tetrahydorfuran-acetic acid （ 51 ： 48 ： 1 ： 0.1 ） as mobile phase. The flow rate was 1 mL· min^-1, the wavelength of UV detector was set at 225 nm and the column temperature was set at 32 ℃. Results： The linear range of evodiamine, rutaecarpine and evodin were 0.015 - 0.3 μg （ r = 0. 999 9）,0.012 - 0.24 μg （ r = 0. 999 9） ,0.059 - 1.18 μg （ r = 0.999 6） respectively. The average recovery of evodiamine was 99.6% （n = 5）, RSD0.65% ; The average recovery of rutaecarpine was 99.1% （ n = 5）, RSD1.2% ; The average recovery of evodin was 97,5% （ n = 5）, RSD 1,4% respectively. Conclusion： This method was simple, rapid and accurate.