HPLC测定胆南星中猪去氧胆酸的含量

目的：建立胆南星中猪去氧胆酸含量测定方法,为其质量控制提供方法。方法：用HPLC-蒸发光散射检测测定样品的猪去氧胆酸含量。色谱和检测条件：Diamonsil C₁₈色谱柱(4.6 mm×250 mm,5 μm),柱温35 ℃；流动相甲醇-水-冰醋酸(75∶25∶0.01),流速1 mL·min^{-1；漂移管温度85 ℃,空气流速3.0 L·min-1。结果：猪去氧胆酸进样量在2.4～24 μg,进样量和峰面积的对数呈线性(r= 0.999 8)。平均加样回收率为97.1%,RSD 3.0%(n=5)。结论：方法简便,测定准确,且重复性好,可用于胆南星的质量控制。}

Determination of chyodeoxycholic acid in Bile Arisaema by HPLC-ELSD

OBJECTIVE: To develop an HPLC method for the determination of hyodeoxycholic acid in Bile Arisaema. METHOD: The methanol extracts were separated on a Diamonsil ODS column eluted at 35 degrees C with a mixture of methanol-water-glacial acetic acid (75:25:0.01) at flow-rate 1.0 mL x min(-1). The drift-tube temperature of ELSD was 85 degrees C, and the flow rate of air was 3.0 L x min(-1). RESULT: Hyodeoxycholic acid in methanol extract was well separated, the relationship of logarithms of injection amount and peak area was linear (r = 0.9998) over the range of 2.4-24 microg. The average recovery was 97.1% (RSD 2.9%, n=5). CONCLUSION: The method could be used for quality control of Bile Arisaema.