摘要
目的建立HPLC法同时测定银黄颗粒中6个咖啡酰奎宁酸类。方法银黄颗粒50%甲醇提取物分析采用Kromasil C18色谱柱（250 mm×4.6 mm,5μm）,以乙腈（A）-0.4%磷酸溶液（B）为流动相,梯度洗脱,柱温35℃,体积流量1.0 m L/min,检测波长327 nm。结果 3-O-咖啡酰奎宁酸、绿原酸（5-O-咖啡酰奎宁酸）、4-O-咖啡酰奎宁酸、4,5-O-二咖啡酰奎宁酸、3,5-O-二咖啡酰奎宁酸和3,4-O-二咖啡酰奎宁酸进样量分别在0.012～0.236μg、0.043～0.866μg、0.013～0.253μg、0.012～0.246μg、0.012～0.248μg和0.020～0.397μg范围内与色谱峰峰面积呈良好的线性关系;平均回收率（n=6）分别为96.2%、96.8%、96.2%、104.9%、96.8%和95.9%;RSD分别为0.6%、0.5%、1.3%、0.4%、0.2%和0.3%。结论 26批银黄颗粒样品的绿原酸含有量差别不大,但其他5个咖啡酰奎宁酸含有量差异较大。建议以咖啡酰奎宁酸类成分代替绿原酸检测银黄颗粒。
AIM To establish an HPLC method for simultaneously determining six caffeoyl quinic acids in Yinhuang Granules.METHODS The analysis of Yinhuang Granules 50% methanolic extract was performed on Kromasil C18column（250 mm × 4.6 mm,5 μm）.The mobile phase was consisted of acetonitrile（A）-0.4%phosphoric acid solution（B） in a gradient elution manner with a flow rate of 1.0 m L / min at 35 ℃.The detection wavelength was set at 327 nm.RESULTS The linear ranges of 3-O-caffeoyl quinic acid,chlorogenic acid（5-Ocaffeoyl quinic acid）,4-O-caffeoyl quinic acid,4,5-O-dicaffeoyl quinic acid,3,5-O-dicaffeoyl quinic acid,and3,4-O-dicaffeoyl quinic acid fell within the ranges of 0.012-0.236 μg,0.043-0.866 μg,0.013-0.253 μg,0.012-0.246 μg,0.012-0.248 μg,and 0.020-0.397 μg,respectively.Their average recoveries（n = 6）were 96.2%,96.8%,96.2%,104.9%,96.8%,and 95.9%,respectively.Their relative standard deviations were 0.6%,0.5%,1.3%,0.4%,0.2%,and 0.3%,respectively.CONCLUSION The HPLC data from inspection of twenty six batches of Yinhuang Granules show that chlorogenic acid content is somewhat different,but other five caffeoyl quinic acids contents present significant different,so suggesting that chlorogenic acid is substituted by caffeoyl quinic acids in the determination of Yinhuang Granules.
出处
《中成药》
CAS
CSCD
北大核心
2015年第2期311-315,共5页
Chinese Traditional Patent Medicine
基金
国家重大新药创制中药质量安全检测和风险控制技术平台(2014ZX09304307-002)
山东省自然科学基金项目(ZR2013HM074)
