辰砂六一散指纹图谱及其含量测定

Study on HPLC fingerprint and content determination of Chensha Liuyi San

目的采用高效液相色谱法建立中药制剂辰砂六一散的指纹图谱,并同时测定其中甘草苷和甘草酸的含量。方法采用Wondasil C_(18)色谱柱(250×4.6 mm,5μm),以乙腈-体积分数0.05%磷酸溶液为流动相进行梯度洗脱,流速为1 mL·min^(-1),检测波长为237 nm,柱温30℃;建立辰砂六一散指纹图谱,运用中国药典委员会"中药色谱指纹图谱相似度评价系统软件"进行相似度评价,并对其中两个色谱峰进行指认及含量测定。结果10批辰砂六一散指纹图谱中标定了共有色谱峰,相似度值为0.981~0.995。甘草苷和甘草酸质量浓度分别在5.0~30.0 mg·L^(-1)和12.6~75.6 mg·L^(-1)内与峰面积呈良好的线性关系,平均回收率分别为99.6%和99.5%。结论该法所建立的指纹图谱方法简便、重复性好、特征性强,结合有关成分的含量测定能更好地控制其质量,对提高辰砂六一散的整体质量控制提供参考依据。

Objective To establish the HPLC fingerprint of Chensha Liuyi San, and to simultaneously determinate the contents of liquiritin and glycyrrhizic acid. Methods The separation was performed on a Wondasil C18 colunm （250 mm × 4. 6 mm, 5 μm） with acetonitrile-water （ containing 0. 05 % phosphoric acid）as the mobile phase by gradient elution at the flow rate of 1.0 mL. min-1. The detection wavelength was 237 nm and the column temperature was 30 ℃. An HPLC fingerprint of Chensha Liuyi San was set up and the quality of 10 batches of Chensha Liuyi San was evaluated by similarity assay. Furthermore,the two of the peaks were identified and the contents were determinated. Results The fingerprint chromatogram had 15 common peaks,and the similarities of 10 batches of Chensha Liuyi San were about 0. 981 to 0. 995. The linear range of liquiritin and glycyrrhizic acid were 5.0 -30. 0 mg. L-1 and 12. 6 -75.6 mg. L-1, respectively. The average recoveries were 99. 6% and 99. 5%, respectively. Conclusions The established method for HPLC fingerprint of Chensha Liuyi San is simple, reproducible and specific, which can be used for the quality evaluation of Chensha Liuyi San combining with the content determination.