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目的建立RP-HPLC测定制川乌中乌头碱、次乌头碱和新乌头碱含量的方法。方法采用Zorbax Eclipse XDB-C8色谱柱(200mm×4.6mm,5μm);以20mmol·L-1三乙胺溶液(磷酸调pH3)-甲醇(95:5)为流动相梯度洗脱;检测波长235nm;柱温30℃;流速1.0mL·min-1。结果三种生物碱得到有效分离,回归方程分别为:Y乌头碱=1.257×104X+0.222(r=0.9999)、Y次乌头碱=1.302×104X+0.293(r=0.9997)、Y新乌头碱=1.295×104X-0.119(r=0.9999);线性范围为:0.5～20.0μg·mL-1;平均加样回收率分别为98.42%、97.51%、98.33%;RSD分别为1.05%、1.07%、1.05%(n=6)。结论所建方法对制川乌中生物碱的含量控制具参考意义。
Objective To establish a RP-HPLC method for the determination of aconitine, hypaconitine and mesaconitine in Radix Aconitum. Methods A Zorbax Eclipse XDB-C8 column (200 mm × 4.6 mm, 5 μm) was used. The mobile phase was eluted with 20 mmol·L -1 Triethylamine (adjusted to pH 3) and methanol (95: 5) ; Column temperature 30 ℃; flow rate 1.0mL · min-1. Results The three alkaloids were effectively separated and the regression equations were: Y aconitine = 1.257 × 104X + 0.222 (r = 0.9999), Y aconitine = 1.302 × 104X + 0.293 (r = 0.9997) The average recoveries were 98.42%, 97.51% and 98.33%, respectively. The RSDs were 1.05% and 1.07, respectively. The linear range was 0.5-20.0μg · mL-1. %, 1.05% (n = 6). Conclusion The proposed method has reference value for the control of alkaloids in Radix Aconiti Preparata.