SPE-HPLC测定风湿马钱片中的马钱子碱

Determination of brucine in Fengshi Maqian tablet by SPE-HPLC

采用固相萃取进行样品前处理,建立固相萃取-高效液相色谱法（SPE-HPLC）测定风湿马钱片中马钱子碱含量的分析方法。采用PXC阳离子交换固相萃取小柱净化,C18（250 mm×4.6 mm,5μm）色谱柱,流动相为乙腈-0.01 mol/L庚烷磺酸钠与0.02 mol/L磷酸二氢钾等量混合溶液（用体积分数为10%的磷酸调节p H值为2.8）,二者体积比为21∶79,流速为1.0 m L/min,检测波长为262 nm,柱温为30℃。结果发现,马钱子碱在40~60μg/m L范围线性关系良好,相关系数为0.9993,平均回收率为99.6%~101.0%,RSD值为1.04%。该方法操作简便、准确,重现性好,适用于风湿马钱片中马钱子碱的含量测定。

To establish the SPE-HPLC method for determining content of brucine in Fengshi Maqian tablet,the cation exchange solid phase extraction column is used to purity the samples. By using PXC cation exchange solid phase extraction（ SPE）,the HPLC column used in the experiment is C18（ 250 mm × 4. 6 mm,5 μm）,the mobile phase consists of acetonitrile-0. 01 mol/L sodium heptanesulfonate and 0. 02 mol / L KH2PO4 mixed half and half（ adjusting p H to 2. 8 with 10% phosphoric acid）（ volume ratio of 21∶ 79）,the flow rate is 1. 0 m L / min,the detection wavelength is 262 nm,and the column temperature is 30 ℃. The content of brucine determined by SPE-HPLC method has good linear relationship with the peak areas when their concentration is at 40 ~ 60 μg / m L（ r = 0. 999 3）. The range of recovery rates of Brucine are 99. 6% ~ 101. 0%（ RSD = 1. 04%）. This method is simple and accurate with good reproducibility,and it can be used to determine the content of brucine in Fengshi Maqian tablet.