战骨药材及其复方制剂的指纹图谱分析及牡荆素含量测定

Fingerprinting Analysis and Content Determination of Vitexin of Premna fulva Craib and Its Compound Preparation

建立战骨药材及其复方制剂的HPLC指纹图谱分析及牡荆素的HPLC含量测定方法,并考察牡荆素在跌打生骨胶囊制备过程中的含量变化。采用Waters Xbridge C18（4.6 mm×250 mm,5μm）色谱柱;流动相为乙腈-0.5%冰醋酸水溶液,梯度洗脱;流速为1.0mL/min;检测波长为350 nm;柱温：25oC。结果表明牡荆素在0.16~0.80μg范围内线性关系良好（R2=0.9996）;10批战骨药材的指纹图谱有19个共有特征峰,其峰面积占总峰面积的90%以上。每克药材含牡荆素在15.8~30.2μg之间。制备胶囊的稠膏及内容物颗粒未检出牡荆素。表明本实验建立的HPLC方法可用于测定战骨药材中牡荆素的含量,而不适用于其复方制剂中牡荆素的含量测定。

The objective of this study was to develop a HPLC method for the fingerprinting analysis of Premnafulva Craib and to determine the content of vitexin in P. fulva and its compound preparation. The chromatographic separation was carried out using Waters Xbridge Cls column （4.6 mm ×250 mm,5 μm） with gradient elution. The mobile phase was comprised of aeetonitrile-0.5% glacial acetic acid in water,the UV detection wavelength was set at 350 nm,with a flow rate of 1.0 mL/min, and column temperature was maintained at 25 ℃. Results showed that good linear relationship of vitexin was achieved in the range of 0.16-0.80 p.g （R2 = 0.9996）. There were 19 common peaks （peak areas account for more than 90% of total peaks） in the fingerprints of 10 batches of P.fulva. The contents of vitexin in 10 batches of P. fulva samples were between 15.8 - 30.2 μg/g. In addition, vitexin was not detected in Dieda Shenggu capsules or extract. Hence, it was concluded that the developed HPLC method can be used as a quality control method for vitexin in P. fulva. While,it was unsuitable for its compound preparation.