HPLC法同时测定苦木注射液中3种活性成分的含量

目的: 建立同时测定苦木注射液中3种活性成分3-甲基-铁屎米-2,6-二酮、4-甲氧基-5-羟基铁屎米酮、4,5-二甲氧基-铁屎米酮含量的分析方法。 方法: 采用高效液相色谱法,色谱柱为Phenomenex Gemini C₁₈(150 mm×4.6 mm,5 μm)柱,流动相为pH 7.5的0.2 mol·L^-1磷酸氢二钠及磷酸二氢钠缓冲液 (A)–甲醇(B),梯度洗脱,流速1 mL·min^-1,检测波长254 nm,柱温30 ℃。 结果: 苦木注射液中3-甲基-铁屎米-2,6-二酮、4-甲氧基-5-羟基铁屎米酮、4,5-二甲氧基-铁屎米酮线性范围分别为0.0380~0.7600 μg(r=0.9999),0.0450~0.9000 μg(r=0.9999),0.0287~0.574 μg(r=0.9999);平均加样回收率(n=9)分别为99.3%,101.4%,101.8%。 结论: 该方法操作简单,重复性好,为评价和监控苦木注射液的质量提供可靠的方法。

Objective: To establish a method for simultaneous determination of three active ingredients:3-methylcanthin-2,6-dione,4-methoxy-5-hydroxycanthin-6-one,4,5-dimethoxycanthin-6-one in Kumu injection. Methods: The determination was carried out with Phenomenex Gemini C₁₈ column(150 mm×4.6 mm,5 μm);The mobile phase consisted of 0.2 mol·L^-1,pH 7.5 phosphate buffer (A)-methanol(B) with gradient elution at a flow rate of 1.0 mL·min^-1;The detection wavelength was 254 nm,and the column temperature was 30 ℃. Results: The calibration curves were linear in the ranges of 0.0380-0.7600 μg for 3-methylcanthin-2,6-dione(r=0.9999),0.0450-0.9000 μg for 4-methoxy-5-hydroxycanthin-6-one(r=0.9999) and 0.0287-0.574 μg for 4,5-dimethoxycanthin-6-one(r=0.9999).The average recoveries(n=9) were 99.3%,101.4%,and 101.8%,respectively. Conclusion :The method is simple and repeatable,which can be applied to the quality control of the Kumu injection.