高效液相色谱法测定嘎日迪五味丸中乌头碱、中乌头碱和次乌头碱含量

摘要

Objective To establish HPLC method for determining the content of aconitine,mesaconitine and hypaconitine in Garidi -5 Pills. Methods The chromatographic column was Symmetry C18 (150 mm × 4. 6 mm, 5 μm) , the mobile phase was methol - water - chloroform - glacial acetic acid - thriethylamine (50 ∶ 50 ∶ 2 ∶ 1 ∶ 0. 6),the column temperature was 25 ℃ , the flow rate of 1. 0 mL/min, the UV detection wavelength was 254 nm. Results The linear range of concentration of three compounds was 9. 0 -45. 0 μg/mL. Regression equations were A1 = 2. 125 × 106 C ＋ 1. 252 × 104 , A2 = 2. 143 × 106 C ＋ 1. 422 × 104 , A3 = 1. 968 × 106 C - 2. 152 × 104 , r were 0. 999 6 , 0. 999 8 , 0. 999 9, respectively. The average recoveries and the relative standard deviation were 100. 40％ ,99. 61％, 100. 15% and 0. 72％ , 0. 86％ ,0. 89％ , respectively. Conclusion The method is simple, fast and accurate. It is suitable for content determination of aconitine, mesaconitine and hypaconitine in Garidi - 5 Pills.%目的 建立测定嘎日迪五味丸中乌头碱、中乌头碱和次乌头碱含量的高效液相色谱法.方法 色谱柱为Symmetry C18柱(150 mm×4.6 mm,5μm),流动相为甲醇-水-氯仿-冰醋酸-三乙胺(50:50:2:1:0.6),柱温为25℃,流速为1.0 mL/min,检测波长为254 nm.结果 乌头碱、中乌头碱和次乌头碱的质量浓度均在9.0～45.0μg/mL范围内与峰面积线性关系良好,回归方程分别为A1=2.125×106C+1.252×104,A2=2.143×106C+1.422×104,A3=1.968×106C-2.152×104,相关系数r分别为0.9996,0.999 8,0.999 8,平均回收率分别为100.40%,99.61%,100.15%,RSD分别为0.72%,0.86%,0.89%.结论 所用方法简便、快速、准确,适用于嘎日迪五味丸中乌头碱、中乌头碱和次乌头碱的含量测定.