固相萃取-反相高效液相色谱法检测木瓜丸中双酯型生物碱限度

Determination of Diester Alkaloid Limit in Mugua Pills by SPE-HPLC

目的建立同时测定木瓜丸中3种双酯型生物碱含量的固相萃取-反相高效液相色谱(SPE-HPLC)法。方法色谱柱采用Eclipse XDB-C_(18)柱(250 mm×4.6 mm,5μm),流动相为0.1%醋酸铵溶液(冰醋酸调pH=3.5)-乙腈(75∶25),流速为1.0 m L/min,检测波长为235 nm,柱温为40℃。结果新乌头碱、乌头碱、次乌头碱质量浓度分别在1.25~12.5μg/m L,3.10~31.0μg/m L,3.24~32.4μg/m L范围内与峰面积线性关系良好;平均加样回收率为98.01%,RSD为1.50(n=6)。结论该方法快速简便,准确可靠,灵敏度高,可用于木瓜丸中3种有毒双酯型生物碱含量测定,以控制药品质量。

Objective To establish an SEP-HPLC method for simultaneous determination of three kinds of diester alkaloids in Mugua Pills. Methods The Eclipse XDB-C18 column （ 250 mm × 4. 6 mm, 5 μm ） was adopted, the mobile phase was 0. 1% ammonium acetate solution （ pH was adjusted to 3. 5 by glacial acetic acid ） - acetonitrile （ 75 ：25 ） , the flow rate was 1. 0 mL/min, the detection wave-length was 235 nm, and the column temperature was 40 ℃. Results The concentrations of new aconitine, aconitine and hypaconitine were in the range of 1. 25-12. 5 μg/mL, 3. 10-31. 0 μg/mL, 3. 24-32. 4 μg/mL, the average recovery was 98. 01% and RSD was 1. 50% （ n=6 ） . Conclusion The method is rapid, simple, accurate, reliable and sensitive. It can be used to determine the contents of three toxic diester alkaloids in Mugua Pills and to control the quality of the drugs.