反相高效液相色谱法测定骨痹灵片中士的宁和马钱子碱的含量

Determination of Strychnine and Brucine in Gubiling Tablets by RP-HPLC

目的采用反相高效液相色谱法测定骨痹灵中士的宁和马钱子碱含量。方法色谱柱为CAPCELL C18（4.6×150mm,5μm）,流动相为乙腈-0.01 mol·L-1庚烷磺酸钠与0.02 mol·L-1磷酸二氢钾等量混合溶液（用10%磷酸调节p H值至2.8）（20：80,V/V）,检测波长为260 nm,柱温为40℃,流速为0.8ml·min-1。结果士的宁进样量在0.047~0.234μg范围内与其峰面积呈良好的线性关系（r=0.999 9）,平均加样回收率99.09%,RSD为0.79%（n=6）;马钱子碱进样量在0.035~0.173μg（r=0.999 7）范围内与其峰面积呈良好的线性关系（r=0.999 7）,平均加样回收率98.54%,RSD为1.02%（n=6）。结论该方法准确、重复性好、灵敏度高,可用于骨痹灵片的质量控制。

Objective To establish an RP-HPLC method for determination of strychnine and brucine in Gubiling tablets. Methods The column was CAPCELL C18（4.6 × 150 mm, 5 μm）, and the mobile phase was acetonitrile- 0.01 mol·L-1 sodium heptanesulfonate mixed with same quantity of 0.02 mol·L-1 potassium dihydrogen（adjusted p H to 2.8 by 10% phosphoric acid）（20：80, V/V）,the detection wavelength was 260 nm,the column temperature was 40 ℃, and the fl ow rate was 0.8ml·min-1. Results The linear range of strychnine was 0.047 ~ 0.234 μg（r = 0.999 9）,the average recovery was 99.09%,and the RSD was 0.79%（n = 6）.The linear range of brucine was 0.035 ~ 0.173 μg（r = 0.999 7）, the average recovery was 98.54%,and the RSD was 1.02%（n=6）.Conclusion The method is accurate, repeatable and sensitive,which can be used for the quality control of Gubiling tablets.