通脉丸溶出液中士的宁和马钱子碱的含量测定  

Determination of the Contents of Strychnine and Brucine in Dissolution Liquid of Tongmai Pills

作　　者：陈天朝[1] 梁启超[2] 李丽[2] 于兰兰[2] 刘瑞霞[2] 

机构地区：[1]河南中医学院第一附属医院,河南郑州450000 [2]河南中医学院,河南郑州450046

出　　处：《中医学报》2016年第4期563-566,共4页Acta Chinese Medicine

基　　金：河南省科技厅自然科学基金项目(102102310185);河南省教育厅项目(13A350597)

摘　　要：目的:建立通脉丸溶出液中士的宁和马钱子碱的含量测定方法。方法:采用超高效液相色谱法测定通脉丸溶出液中士的宁和马钱子碱的含量,色谱条件:Acquity UPLC BEH C_(18)(2.1 mm×100 mm,1.7μm)色谱柱,以乙腈-0.02 mol·L^(-1)磷酸二氢钾与0.014 8 mol·L^(-1)庚烷磺酸钠等量混合溶液(用体积分数10%磷酸调节PH为2.8)(17∶83)为流动相;检测波长为260 nm;流速为0.3 m L·min^(-1);柱温30℃。结果:本方法对通脉丸溶出液中士的宁与马钱子碱均能适用,其中马钱子碱在3.712~74.24μg、士的宁在3.472~69.44μg内呈良好线性关系,r^2=0.999 9,平均加样回收率分别为102.65%(RSD 1.08%),104.19%(RSD 1.46%)。结论:该法分离效果好,专属性强,操作简便快捷,适用于通脉丸溶出液中马钱子碱与士的宁的测定。Objective：To establish the UPLC method for determination of strychnine and brucine in dissolution liquid of Tongmai pills. Methods：UPLC was performed on a BEH C18（2. 1 mm × 100 mm,1. 7 μm）. The mobile phase consisted of 17% acetonitrile and 83% water containing 0. 02 mol·L-1potassium dihydrogen phosphate and 0. 0148 mol·L-1sodium heptanes sulfonate（ adjusting PH 2. 8 with 10% phosphonic acid）. The detection wavelength was set at 260 nm. The flow rate was 0. 3 m L·min-1. The column temperature was 30 ℃. Results：The chromatographic conditions for the dissolution fluid of tongmai pills Strychnine and brucine can apply. The calibration curves were linear within the range of 3. 712- 74. 24 μg for brucine,3. 472- 69. 44 μg for strychnine,r2= 0. 999 9,average recoveries of these two components were 102. 65%（ RSD 1. 08%）,104. 19%（ RSD 1. 46%）,respectively. Conclusion：This established quantitative analysis is improved by pharmacopoeia method,reliable and accurate,UPLC is reliable,simple and precise,which are suitable for quality control of strychnine and brucine in dissolution liquid of Tongmai pills.

关 键 词：通脉丸 马钱子碱 士的宁 超高效液相色谱法 

分 类 号：R284.2[医药卫生—中药学]