南方医科大学学报

南方医科大学学报 ›› 2006, Vol. 26 ›› Issue (10): 1503-1505.

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复方蒲公英灌肠液指纹图谱定性和有效成分定量分析方法研究

李亦蕾； 晏媛； 谭亚非； 许重远； 陈志良；   

  1. 南方医科大学南方医院药学部； 南方医科大学南方医院药学部 广东广州510515； 广东广州510515；
  • 出版日期:2006-10-20 发布日期:2006-10-20

Qualitative fingerprint and quantitative determination of caffeic acid in compound dandelion enema

LI Yi-lei, YAN Yuan, TAN Ya-fei, XU Zhong-yuan, CHEN Zhi-liang Department of Pharmacy, Nanfang Hospital, Southern Medical University, Guangzhou 510515, China   

  1. 南方医科大学南方医院药学部； 南方医科大学南方医院药学部 广东广州510515； 广东广州510515；
  • Online:2006-10-20 Published:2006-10-20

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摘要： 目的运用指纹图谱技术建立复方蒲公英灌肠液的反相高效液相色谱(RP-HPLC)定性和定量方法,为科学评价及有效控制其质量提供可靠方法。方法利用RP-HPLC方法,梯度洗脱测定10批样品。色谱条件为:HypersilBDSC18分析柱(5μm,250mm×4.6mm);流动相A为乙腈,流动相B为磷酸盐缓冲液(磷酸调pH为3.2),流动相A梯度洗脱(10%-80%乙腈),分析时间40min,时间为0、38、40min,A(%)为10%、80%、80%;柱温35℃;流速:0.7ml/min;检测波长:254nm。结果10批复方蒲公英灌肠液样品得到的色谱指纹图谱有23个共有峰,可作为定性鉴别的指标峰;通过与标准品的保留时间及紫外光谱比较,3、4和8号峰分别鉴定为原儿茶醛、咖啡酸和阿魏酸,复方蒲公英灌肠液中咖啡酸的含量为(63.7-136.8)μg/ml。结论复方蒲公英灌肠液的指纹图谱特征性和专属性强,可结合咖啡酸的含量测定用于全面控制产品的质量。 

Abstract: Objective To establish a qualitative and quantitative reversed-phase high-performance liquid chromatography (RP-HPLC) with fingerprinting technique for quality control of compound dandelion enema. Methods HPLC was utilized for quality assessment of 10 batches of samples. RP-HPLC analysis was performed on a Hypersil BDS C18 column (4.6 mm×250 mm, 5 μm) with the mixture of acetonitrile (A) and potassium phosphate solution (B) (pH3.2) as the mobile phase in gradient mode. The concentrations of solvent A were 10%, 80% and 80% at 0, 38 and 40 min, respectively. The column temperature was set at 35 ℃, the flow rate at 0.7 ml/min and the detection wavelength at 254 nm. Results HPLC fingerprinting was established from the 10 batches, and the data showed 23 characteristic peaks in the compound dandelion enema for use as index peaks for qualitative identification. Comparison of the retention time and the on-line UV spectra of the samples with the chemical standards identified peaks 3, 4 and 8 as protocatechualdehyde, caffeic acid and ferulic acid, respectively. The contents of caffeic acid in the compound dandelion enema ranged between 63.7 and 136.8 μg/ml. Conclusion High specific chromatographic fingerprinting and quantitative measurement of caffeic acid allows rigorous quality control of compound dandelion enema. 

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