苦木药材中3种有效成分的含量测定

Content Determination of Three Effective Constituents in Picrasmae Ramulus et Folium

目的:建立苦木药材中3-甲基-铁屎米-5,6-二酮、4-甲氧基-5-羟基铁屎米酮以及4,5-二甲氧基-铁屎米酮3种生物碱的含量测定方法。方法:用phenomenex Gemini C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-乙酸铵缓冲盐(25 mmol.L-1,冰乙酸调pH 4.0)为流动相,采用梯度洗脱,检测波长为254 nm。结果:3-甲基-铁屎米-5,6-二酮等3种对照品分别在0.004 56～0.182 40,0.012～0.480,0.002 6～0.104 0μg线性良好(r≥0.999 9),平均回收率均>96.72%(RSD<0.78%)。结论:含量测定方法简便、稳定、重复性好,为苦木药材质量控制和评价提供了可靠的方法。

Objective： To establish a method for determination of the content of three alkaloids 3-methyl- canthin-5, 6-dione, 4-methoxy-5-hydroxycanthin-6-one and 4, 5-dinethoxycanthin-6-one in Picrasmae Ramulus et Folium. Method： The determination was carried out with Phenomenex Gemini Cls column （4.6 mm ×250 mm, 5 μm）. The mobile phase consisted of 0.25 mmol· L^-1 ammonium acetate buffer （pH 4.0 by HAC） （A） - acetonitrile （B） with gradient elution. The detection wavelength was at 254 nm. Result： 3-methyl-canthin-5, 6- dione, three reference substances were in good linearity between 0. 004 56-0. 182 40, 0. 012-0. 480, 0. 002 6- 0. 104 0 μg （r≥0. 999 9） , and the average recovery was greater than 96.72% （RSD 〈0.78% ）. Conclusion： The determination method is simple and convenient, stable and repeatable, it would provided a reliable approach to evaluate and control the quality of Picrasmae Ramulus et Folium.