马钱子粉中士的宁和马钱子碱含量测定方法的研究

 目的 通过研究，建立可操作性更强的马钱子粉中指标成分的含量测定方法及限度范围。方法 以十八烷基硅烷键合硅胶为填充剂；以乙腈-水（38∶62），每1 000 mL中含磷酸二氢钾3.4 g和十二烷基硫酸钠1.7 g为流动相；检测波长为260 nm；理论板数按士的宁峰计算应不低于5 000。结果 以干燥品计，10批不同批号的马钱子粉中士的宁的平均含量为0.86%，马钱子碱的平均含量为0.63%，10批样品士的宁的组间平均误差（绝对值）为11.50%。以干燥品计，同一批号10份马钱子粉样品中士的宁的平均含量为0.83%，马钱子碱的平均含量为0.69%，10份样品士的宁的组内平均误差（绝对值）为7.88%。结论 根据马钱子粉制备和测定两个环节的累积总误差（约20%），建议将马钱子粉中士的宁的限度范围修订为：按干燥品计算，含士的宁应为0.64％～0.96％；而马钱子碱仍定为不得少于0.50%。这既可保证马钱子粉的有效与安全，又可大大提高马钱子粉制备过程中的可操作性。

Determination of Strychnine and Brucine in Semen Strychni Pulveratum by HPLC Assay

OBJECTIVE To optimize a HPLC assay for determination of index components in semen strychni pulveratum and establish the linearity range for Chinese Pharmacopoeia (2010). METHODS Octadecyl silane chemically bonded silica was used as bulking agent. The mobile phase consisted of acetonitrile-water (38∶62， contains potassium dihydrogen phosphate 3.4 g and sodium laurylsulate 1.7 g in 1 000 mL ). The detection wavelength was at 260 nm. The theoretical plates were over 5 000 according to Strychnine. RESULTS The average strychnine content in 10 different batch numbers of semen strychni pulveratum was 0.86% and brucine was 0.63%(calculated on the dried basis).The average error between groups of strychnine was 11.5%.The average strychnine content in 10 different samples of the same batch numbers of semen strychni pulveratum was 0.83% and brucine was 0.69%(calculated on the dried basis). The average error within group of strychnine was 7.88%. CONCLUSION Basing on the total error of preparation and determination (about 20%)， the limit range of strychnine was 0.64%-0.96%，and the content of brucine was more than 0.50%. The method improves the efficiency and safety of semen strychni pulveratum and makes it more operable for preparation.