十三味马钱子丸中士的宁和马钱子碱的HPLC测定

Determination of Strychnine and Brucine in ShiSanWei MaQianZi Pill by HPLC

目的：建立一种同时测定十三味马钱子丸中士的宁和马钱子碱的高效液相色谱法。方法：采用高效液相法在同一色谱条件，Dikma C18（4.6 mm×250 mm，5μm）色谱柱；流动相为乙腈-0.01 mol/L庚烷磺酸钠与0.02 mol/L磷酸二氢钾等量混合溶液（用10%磷酸调节pH值2.8）（10：90）；检测波长为260 nm；柱温为30℃；流速为1.0 mL/min；对十三味马钱子丸中两种成分同时进行测定。结果：士的宁、马钱子碱分别在0.262～1.310μg（r=0.9998）、0.172～0.860μg（r=0.9995）线性关系良好。两者的平均回收率分别为97.96%（RSD为1.95%）、98.06%（RSD为2.01%）。结论：所建立的方法简便、专属、重复性好，可用于十三味马钱子丸的质量控制。

Objective：To establish a method for determinate strychnine and brucine in ShiSanWei MaQianZi pill simultaneously by HPLC. Methods：HPLC was adopted under the same condition, Dikma C18（4.6 mm×250 mm, 5 μm） chromatographic column; mobile phase： acetonitrile-0.01mol/L sodium heptanesulfonate and 0.02mol/L potassium dihydrogen phosphate mix solution （regulating pH value 2.8 with 10%phosphoric acid） （10：90）;detec-tion wavelength was 260nm; column temperature： 30℃; flow rate was 1.0mL/min; two kinds of ingredients in ShiSanWei MaQianZi pill were determined simultaneously. Results：Strychnine and brucine showed better linear re-lationship in the ranges between 0.262 and 1.310μg （r=0.999 8）, 0.172 and 0.860μg （r=0.999 5）. Average recovery rates of both were 97.96%（RSD=1.95%）, and 98.06%（RSD=2.01%） respectively. Conclusion：The method, simple, exclusive and good repeatability, could be used for quality control of ShiSanWei MaQianZi pill.