HPLC法测定颈舒片中士的宁和马钱子碱的含量

Determination of Strychine and Brucine in Jingshu Tablets by HPLC

目的：建立颈舒片中士的宁和马钱子碱的含量测定方法。方法以乙腈-0.01mol· L·-1庚烷磺酸钠与0.02mol· L -1磷酸二氢钾等量混合液（用磷酸调pH至2.6）（19∶81）为流动相，柱温：30℃；检测波长260nm，流速0.9mL· min -1。结果士的宁在11.2～179.2μg· mL -1、马钱子碱在10.6～169.6μg· mL -1浓度范围内线性良好，相关系数分别为 r＝0.9999、r ＝0.9990，回收率分别为98.2％、RSD ＝0.74％，99.8％、RSD＝1.4％。结论本法专属性强，操作简便，可作为腰腿痛片的质量控制方法。

OBJECTIVE To establish a method for the determination of Strychine and Brucine in Jingshu Tab-lets by HPLC.METHODS The samples were separated on a Hypersil Gold C18（4.6mm ×150mm,5μm）column at the flow rate of 0.9mL· min-1 and the column temperature was 30℃.Acetonitrile and a mixed solution of equal a-mount of 0.01 mol· L-1 Sodium heptanesulfonate and 0.02 mol · L-1 potassium dihydrogen phosphate （ pH was ad-justed to 2.6 by phosphoric acid ） （ 1∶81 ） was used as the mobile phase , the detection wavelength was 240 nm.RESULTS The method had good linear relationship within the range of 11.2 -179.2μg · mL-1 （ r =0.9999 ） for Strychnine , and 10.6 -169.6μg · mL-1 （ r=0.9998 ） for Brucine.The average recoveries and RSD were 98.2%and 0.74%（ n =9 ） for Strychnine , 99.8%and 1.4%（ n =9 ） for Brucine.CONCLUSION The method is specific ,well-done and can be used for the quality control of Jingshu Tablets.