Pub Date : 2015-04-01DOI: 10.7535/hbkd.2015yx02010
Zetong Wang, Shaomei Wu, Yali Zhang, Yun Ran, Shan Zhang, J. Ha
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.
采用阳离子交换固相萃取柱对样品进行纯化，建立了风石麻千片中马钱子碱含量的SPE-HPLC测定方法。采用PXC阳离子交换固相萃取(SPE)，色谱柱为C18(250 mm × 4)。6 mm,5 μm)，流动相为乙腈-0。01 mol/L庚烷磺酸钠和0。2 mol / L KH2PO4混合一半和一半(调整ph为2)。(体积比为21∶79)，流速为1。0 m L / min，检测波长262 nm，柱温30℃。hplc法测定的马钱子碱含量在40 ~ 60 μg / m L范围内与峰面积呈良好的线性关系(r = 0。3).马钱子碱的回收率范围为99。6% ~ 101。0%(RSD = 1)。04%)。该方法简便、准确，重现性好，可用于风石麻千片中马钱子碱的含量测定。
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