高效液相色谱法同时测定马黄酊中士的宁、马钱子碱和小檗碱的含量  

Simultaneous determination of strychnine,brucine and berberine in Mahuang tincture by HPLC

作　　者：马秋菊[1] 任佳佳[1] 褚志杰[1] 牛韬[1] 马飞[1] 

机构地区：[1]山东中医药大学附属医院,山东济南250011

出　　处：《中国医院药学杂志》2014年第19期1684-1687,共4页Chinese Journal of Hospital Pharmacy

基　　金：山东中医药大学附属医院2013年院级课题

摘　　要：目的：采用HPLC法同时测定马黄酊中士的宁、马钱子碱和小檗碱的含量。方法：HPLC色谱条件,Aglient zorbax SB-C18色谱柱（4.6 mm×150 mm,5μm）,流动相为乙腈（A）-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%磷酸调节至pH2.8）（B）,梯度洗脱,流速1.0ml·min-1,检测波长为260 nm,柱温40℃。结果：3种成分在上述条件下分离良好,士的宁、马钱子碱、小檗碱分别在14.74-58.98μg·ml-1（r=0.999 8）,12.66-50.64μg·ml-1（r=0.999 8）,28.78-115.14μg·ml-1（r=0.999 7）范围内与峰面积线性关系良好,平均回收率（n=6）分别为99.85%,RSD=0.84%;101.59%,RSD=1.05%;98.66%,RSD=0.78%。结论：该方法简便、准确、重复性好,可作为该产品质量控制的方法。OBJECTIVE To establish a method for simultaneous determination of strychnine, brucine and berberine in Mahuang tincture. METHODS A HPLC method was developed for simultaneous determination of strychnine, brucine and berberine in Mahuang tincture. The samples were separated on a Aglient zorbax SB-C18 column （4. 6 mm× 150 mm, 5 μm ）. The mobile phase consisted of acetonitrile （A）-0. 0/ mol.L-1 sodium heptanesulfonate and 0. 02 mol.L -1 potassium d/hydrogen phosphate equivalent volume mixture（B） （adjusted to pH 2. 8 with 10% phosphoric acid） in gradient elution, the flow rate was kept at 1.0 ml. min-1, the detecting wavelength was set at 260 nm, the column temperature was 40 ℃. RESULTS The results indicated that the three compounds were basically isolated. The linear ranges of strychnine and brucine and berberine were 14. 74 - 58.98μg·m1-1 （r= 0. 999 8） ,12. 66 - 50. 64μg·ml-1 （r= 0. 999 8） and 28. 78 - 115.14μg·ml-1 （r= 0. 999 7） respectively. The average recoveries （n = 6） were 99. 85%, 101.59% and 98.66% with RSDs of 0. 84%, 1.05% and 0. 78%, respectively. CONCLUSION The method is simple, accurate and reliable for the quality control of Mahuang tincture.

关 键 词：马黄酊 士的宁 马钱子碱 小檗碱 高效液相色谱法 梯度洗脱 

分 类 号：R927[医药卫生—药学]