HPLC法同时测定复方双金感冒颗粒中3种活性成分的含量

目的: 建立高效液相色谱法同时测定复方双金感冒颗粒(金银花、金莲花、板蓝根、一枝蒿、桑叶等)中荭草苷、牡荆苷、一枝蒿酮酸3种活性成分的含量。方法: 采用Shim-pack VP-ODS色谱柱(250 mm×4.6 mm,5 μm),以乙腈(A)-0.4%磷酸(B)为流动相,梯度洗脱[0~38 min,A-B(14:86),38~60 min,A-B(40:60),60~70 min,A-B(14:86)],流速1 mL·min^-1,柱温30℃,检测波长340 nm(检测荭草苷和牡荆苷)、242 nm(检测一枝蒿酮酸)。结果: 荭草苷、牡荆苷、一枝蒿酮酸质量浓度分别在16.23~97.39、5.154~68.72、9.240~55.44 μg·mL^-1范围内均呈良好线性关系,相关系数分别为0.999 9、0.999 8、0.999 8;平均回收率(n=9)分别为99.45%、100.6%、99.89%,供试品溶液在24 h内稳定。样品中荭草苷、牡荆苷、一枝蒿酮酸含量分别为2.703~2.712、0.338~0.344、0.736~0.742 mg·g^-1。结论: 该方法简便、稳定、可靠可用于同时测定复方双金感冒颗粒中荭草苷、牡荆苷和一枝蒿酮酸的含量,为其质量控制提供保证。

Objective: To establish an HPLC method for simultaneous determination of orientin, vitexin and rupestonic acid in compound Shuangjin Ganmao granules (Lonicera japonica Thunb., Trollius chinensis Bunge, Isatis indigotica Fort., Artemisia rupestris L., and, Morus alba L.etc.). Methods: The determination was carried out on a Shim-pack column (250 mm×4.6 mm, 5 μm)with the column temperature maintained at 30℃.The mobile phase consisted of acetonitrile(A)-0.4% phosphoric a cid (B)solution with the gradient elution [0-38 min, A-B(14:86), 38-60 min, A-B(40:60), 60-70 min, A-B(14:86)].The flow rate was 1 mL·min^-1 and detection wavelength was set at 340 nm (detecting orientin and vitexin)and 242 nm (detecting rupestonic acid). Results: The method Showed good linear relationship within the range of 16.23-97.39 μg·mL^-1 for orientin(r=0.999 9), 5.154-68.72 μg·mL^-1 for vitexin (r=0.999 8) and 9.240-55.44 μg·mL^-1 for rupestonic acid (r=0.999 8), respectively;the average recoveries were 99.45% for orientin, 100.6% for vitexin and 99.89% for rupestonic acid, respectively.The sample solution was stable within 24 h.The contents of orientin, vitexin and rupestonic acid in 3 samples were 2.703-2.712 mg·g^-1, 0.338-0.344 mg·g^-1 and 0.736-0.742 mg·g^-1. Conclusion: The established method is simple, accurate and sensitive, which can be used for the determination of the three components in compound Shuangjin Ganmao granules and is helpful for quality control.