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目的:建立痹通药酒中新乌头碱、次乌头碱、乌头碱的HPLC含量测定方法。方法:Agela Promosil-C18(4.6 mm×250 mm,5μm)色谱柱,柱温35℃,流动相乙腈-四氢呋喃(25∶15)为流动相A,以0.1 moL.L-1醋酸铵溶液(每1 000 mL加冰醋酸0.5 mL)为B,梯度洗脱,流速1.0 mL·min-1,检测波长235 nm。结果:新乌头碱在0.118 9～0.990 9μg呈良好的线性关系(r=0.999 9),平均加样回收率98.07%,RSD1.7%;次乌头碱在0.074 5～0.621 0μg呈良好的线性关系(r=0.999 9),平均加样回收率99.08%,RSD1.5%;乌头碱在0.009 4～0.078 3μg呈良好的线性关系(r=0.999 9),平均加样回收率98.32%,RSD 2.0%。结论:本方法稳定易行、重复性好,可用于痹通药酒质量评价。
Objective: To establish a HPLC method for the determination of mesaconitine, hypaconitine and aconitine in Bi-Tong Liquor. The mobile phase A was acetonitrile-tetrahydrofuran (25:15) as mobile phase A. The mobile phase consisted of 0.1 mol·L-1 ammonium acetate solution 1 mL and glacial acetic acid 0.5 mL) as B, gradient elution, flow rate 1.0 mL · min-1, detection wavelength 235 nm. Results: The new aconitine had a good linearity (r = 0.999 9) between 0.118 9 and 0.990 9 μg with an average recovery of 98.07% and RSD 1.7%. Hypaconitine at 0.074 5 ~ 0.621 0 μg showed good (R = 0.999 9). The average recovery was 99.08% and RSD was 1.5%. Aconitine showed a good linearity (r = 0.999 9) with 0.009 4 ~ 0.078 3 μg. The average recoveries were 98.32% , RSD 2.0%. Conclusion: The method is stable and easy to operate with good repeatability and can be used to evaluate the quality of Bi Tong medicine.