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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 3-methyl-iron-um-5,6-dione, 4-methoxy-5-hydroxy iron-umbelliferone and 4,5-dimethoxy-iron umbelliferone Determination of three alkaloids content. METHODS: The mobile phase consisted of phenomenex Gemini C18 column (4.6 mm × 250 mm, 5 μm) with acetonitrile-ammonium acetate buffer (25 mmol·L-1, glacial acetic acid adjusted to pH 4.0) and gradient elution. The detection wavelength 254 nm. Results: The three reference products of 3-methyl-iron-femi-5,6-dione showed good linearity (r≥0.999 9) at 0.004 56 ~ 0.182 40,0.012 ~ 0.480,0.002 6 ~ 0.104 0μg Rates were> 96.72% (RSD <0.78%). Conclusion: The assay method is simple, stable and reproducible. It provides a reliable method for the quality control and evaluation of bitter wood medicinal materials.