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作 者:易宇阳[1] 赖正权[1] 石书江[1] 陈海明[1] 孔松芝[1] 黄思涵[1] 苏子仁[1,2]
机构地区:[1]广州中医药大学新药开发研究中心,广州510006 [2]东莞广州中医药大学中医药数理工程研究院,广东东莞523808
出 处:《中国实验方剂学杂志》2012年第12期71-74,共4页Chinese Journal of Experimental Traditional Medical Formulae
基 金:国家自然科学基金项目(U0732004)
摘 要: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.
关 键 词:苦木 3-甲基-铁屎米-5 6-二酮 4-甲氧基-5-羟基铁屎米酮 4 5-二甲氧基-铁屎米酮 高效液相色谱法
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